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Forum Description: Discuss the technical details of the preparation of drugs
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Old 10-26-2005, 10:27 AM   #31
kiss_the_cook
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The disadvantages of this method are twofold. First, hydrazine is a
carcinogen. The chemist must wear gloves while doing the reaction, and do a
careful clean-up when finished. If any should be spilled on the skin, a
serious, prolonged, and immediate shower is called for. Care must further
be taken that the fumes of hydrazine are not breathed in, as this could
cause the same problem. Ever try giving your lungs a shower? The other
disadvantage to using this method is that the free bases must be used. This
necessitates the free basing and distillation procedure described in Method
1.
The mechanism by which this procedure works involves first the
formation of a hydrazone by reaction between the ephedrine and hydrazine.
Then at the high temperatures at which this reaction is done, the hydrazone
loses nitrogen (N2) to form meth. This is illustrated:
To do the reaction, a 3000 ml round bottom flask is placed on a buffet
range, and then 1500 ml of diethylene glycol and 336 grams of KOH
(potassium hydroxide) pellets are put in the flask. Next a condenser is
attached to the flask, and water flow is begun through it. Gentle heating
of the flask is now begun, with occasional swirling of the flask to try to
dissolve the KOH pellets. The operator must be ready here to quickly remove
the buffet range, because once the solution warms up, and the KOH pellets
start to dissolve, a great amount of heat is released which could cause the
solution to boil wildly and squirt out the top of the condenser. Since
diethylene glycol has a boiling point of 245C, this would definitely not
be good stuff to be splashed with. Eye protection is, of course, necessary.
The heat source is periodically removed, and then reapplied until the
dissolution of the KOH pellets is complete.
Once the KOH pellets have dissolved, the heat is removed, and the
temperature of the solution is allowed to fall to about 80C. Then 300 ml
of hydrazine hydrate (85% to 100% pure material is OK) and either 303 grams
of PPA free base or 332 grams of ephedrine free base is added to the flask.
The condenser is then immediately replaced, and the mixture is heated with
great caution until any exothermic (i.e. heat generating) reaction has
passed. Then stronger heat is applied to maintain gentle boiling for one
hour.
Now heating is stopped, and as soon as boiling ceases, the condenser is
removed, and the flask is rigged for simple distillation as shown in Figure
3 in Chapter 3. The stillhead should have a thermometer in it reaching down
into the middle of the liquid mass in the flask. A cork or rubber holder
for this thermometer is unacceptable because hydrazine attacks these
materials. The holder must be made of all glass.
Now the heat is reapplied, and distillation is commenced sufficiently
slowly that the froth does not rise out of the flask. Froth can be broken
up by occasional application of weak vacuum, as mentioned back in Chapter
5. When the temperature of the liquid has reached 200C or so (around 200
ml of distillate will have been collected by that point), the heating is
stopped. Once boiling ceases, the stillhead is removed, and the condenser
is reinserted into the flask. Now heat is reapplied, and the mixture is
boiled gently for 3 additional hours.
The reaction is now complete, and it is time to get the product. The
heating is stopped on the flask, and once it has cooled down, the contents
of the flask are poured into 2000 ml of water. The 200 ml of distillate
obtained earlier is also poured into the water. This mixture is stirred to
get the hydrazine out of the meth layer which floats on the top, and into
the water. The solution of KOH in water makes the water fairly hot. Once it
has cooled down, 500 ml of toluene is added, and the mixture is shaken. A
one gallon glass jug is a good vessel to do this in. The top layer of meth
dissolved in toluene is then separated, and distilled as described earlier.
The yield is 250 to 275 ml of meth. If a careful fractional distillation is
not done, the product may be contaminated with a small amount of hydrazine.
This is definitely not good, and may be avoided by shaking the separated
meth dissolved in toluene layer with a fresh portion of water.
Method 3: Direct Reduction of Ephedrine With Palladium
This method is very similar to the indirect reduction of ephedrine. The
difference in this case is that here the chlorination and reduction are
done simultaneously in a "one pot" process. This has the obvious advantages
of being quicker and using fewer chemicals. This method has the further
advantage of using ephedrine, pseudoephedrine, or PPA in their
hydrochloride or sulfate salt forms, so no free basing or distilling of the
raw material inputs is needed. Another advantage is that the chlorination
is done using dry HCl gas Since this is easily made from dripping sulfuric
acid on table salt, the chemist need never worry about having to get
suspicion-arousing chemicals to maintain production.
There are a couple of drawbacks to the use of this method. First and
foremost, the contents of the hydrogenation bomb must be heated to about
80-90C during the reaction. This leads to a possible danger whereby the
champagne bottle hydrogenation bomb may crack and burst due to heat stress.
This is a possibility even if it is coated on the outside with fiberglass
resin. Another drawback is the need to invest in about $1000 worth of
palladium chloride to begin production. The catalyst prepared from this
palladium chloride can be used over and over again, but it is still a
considerable initial cost.
To do this reaction, the chemist first prepares palladium black
catalyst. This is done as follows: In a 2000 ml beaker, 50 grams of
palladium chloride is dissolved in 300 ml of concentrated hydrochloric acid
(laboratory grade, 35-37%). Once it has all dissolved, it is diluted with
800 ml of distilled water. Next, the beaker is nestled in a bed of ice that
has been salted down. This is an ice-salt bath. The contents of the beaker
are stirred occasionally, and once it is cold, 300 ml of 40% formaldehyde
solution is added with stirring. After a few minutes, a cold solution of
350 grams KOH in 350 ml distilled water is added slowly over a period of 30
minutes. The palladium solution must be vigorously stirred during the
addition. Now the beaker is removed from the ice, and warmed it up to 60
for 30 minutes with occasional stirring during the heating.
When the heating is complete, the beaker is set aside to cool, and for
the catalyst to settle. Once the catalyst has settled, the chemist pours
off as much of the water solution as possible, without losing any catalyst.
Then fresh distilled water is added to the beaker, the catalyst is stirred
up to wash it off, then the chemist lets it settle again, and pours off the
water. This washing is repeated a total of six times. Finally, the catalyst
is suspended in a bit of fresh distilled water, and filtered, preferably
through sintered glass to be sure of catching all the catalyst. Any
catalyst still clinging to the sides of the beaker are rinsed down with
water and poured in with the main body of catalyst. It is wise to rinse off
the catalyst again with still another large portion of water while it is in
the filtering funnel. This process yields 31 grams of palladium black
catalyst, once it has dried. It is important that the catalyst be allowed
to dry completely, because the presence of water in the reaction mixture is
to be avoided.
With a supply of catalyst on hand, the chemist can move on to
production. To begin, 600 ml of glacial acetic acid is poured into a 1000
ml beaker. Now the glassware is set up as shown in Figure 10 back in
Chapter 5. The glass tubing is lead into the acetic acid, and bubbling of
dry HCl gas into the acetic acid is begun as described in that chapter. It
is a good idea here to magnetically stir the acetic acid solution during
the bubbling. The whirlpool formed will help the bubbles of HCl gas to
dissolve in the acetic acid, rather than escape and waft away on the
breezes. This bubbling is continued until the acetic acid solution has
gained 30 grams in weight.
Next, this acetic acid-HCl mix is poured into the 1.5 liter champagne
bottle hydrogenation device along with 60 grams of either ephedrine,
pseudoephedrine or PPA (sulfate or HCl salt OK for any of these), and 50
grams of palladium catalyst. Since the mixture is going to be magnetically
stirred, a magnetic stirring bar, of course, is put in the bottle. Now the
apparatus is set up as shown in Figure 17 in Chapter 11. The air is sucked
out of the bottle as described in that chapter, and replaced with hydrogen.
Pressure is avoided for now until the heating of the bottle contents is
well underway. To heat the bottle contents, it is best to use a steam
cabinet. One can best make such a cabinet from a styrofoam cooler. (See
Figure 22).
The chemist simply leads steam from a pressure cooker into the
styrofoam party cooler via automotive vacuum tubing. The lid is on the
cooler, with a small hole in the lid of the cooler for the top of the
bottle to stick out of, or for the hydrogen line to get in through. It is
best to poke a small hole in the side of the cooler near the bottom, and
stick some plastic tubing into it. This acts as a drain line to carry away
condensed water.
Now the chemist begins stirring, and once the bottle has warmed up a
bit, increases pressure to the 15 to 30 pound range. In about an hour, the
reaction is finished. The chemist can tell this because it stops absorbing
hydrogen. The heating is then stopped, and the stirring is halted. The
hydrogen is vented outside as described back in Chapter 11, and the product
solution is carefully poured out of the bottle, taking care not to pour out
the palladium catalyst. If any comes out, it is filtered, and the palladium
returned to the bottle for the next run.
The product mixture is poured into a 1000 ml round bottom flask along
with a few pumice chips, and the glassware is set up as shown in Figure 3.
The chemist distills off 500 ml of acetic acid (b.p. 118C). This acetic
acid can probably be used over a few times in the reaction. Eventually,
water will build up in it, rendering it useless.
The residue left in the distilling flask has the product. Once it has
cooled down, lye water is added to it, and shake vigorously. The solution
should be strongly basic. Now toluene is added, the top layer separated
off, and this top layer is distilled as described so often in this book to
yield a little over 50 grams of meth (or benzedrine if PPA was used). This
is
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Old 10-26-2005, 10:28 AM   #32
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about 95% yield.
A variety of other acids besides HC1 can be used to do this reaction.
Sulfuric, phosphoric, and perchloric acids will all form esters with the
alcohol grouping of ephedrine, pseudoephedrine or PPA, and this ester can
be reduced to yield meth or plain amphetamine. See Chem Abstracts, Volume
34, column 3761, also Volume 38, column 1219 and Volume 34, column 7297.
Also see J. Med. Chem., Volume 9, page 996.
Method 4: Reduction With Hydroiodic Acid and Red Phosphorus
In this procedure, the alcohol grouping of ephedrine, pseudoephedrine,
or PPA is reduced by boiling one of these compounds in a mixture of
hydroiodic acid and red phosphorus. Hydroiodic acid works as a reducing
agent because it dissociates at higher temperatures to iodine and hydrogen,
which does the reducing. This dissociation is reversible. The equilibrium
is shifted in favor of dissociation by adding red phosphorus to the
mixture. The red phosphorus reacts with the iodine to produce PI3, which
then further reacts with water to form phosphorus acid and more hydroiodic
acid. Since the hydrogen atom of the HI is being absorbed by the ephedrine,
the red phosphorus acts as a recycler.
In some reductions, the need for HI is dispensed with just by mixing
red phosphorus and iodine crystals in a water solution. The red phosphorus
then goes on to make HI by the above mentioned process. With a small amount
of due care, this is an excellent alternative to either purchasing,
stealing, or making your own pure hydroiodic acid.
This method has the advantage of being simple to do. It was formerly
the most popular method of making meth from ephedrine. Now red phosphorus
is on the California list of less restricted chemicals, so an increased
level of subterfuge is called for to obtain significant amounts. One might
think that this is easily gotten around by making your own red phosphorus,
but this is a process I would not want to undertake. Ever hear of
phosphorus shells? I would much rather face the danger of exploding
champagne bottles. Those who insist upon finding out for themselves, will
see Journal of the American Chemical Society, volume 68, page 2305. As I
recall, The Poor Man's James Bond also has a formula for making red
phosphorus. Those with a knack for scrounging from industrial sources will
profit from knowing that red phosphorus is used in large quantities in the
fireworks and matchmaking industries. The striking pad on books of matches
is about 50% red phosphorus.
The determined experimenter could obtain a pile of red phosphorus by
scraping off the striking pad with a sharp knife. A typical composition of
the striking pad is about 40% red phosphorus, along with about 30% antimony
sulfide, and lesser amounts of glue, iron oxide, MnO2, and glass powder. I
don't think these contaminants will seriously interfere with the reaction.
Naturally, it is a tedious process to get large amounts of red phosphorus
by scraping the striking pad off matchbooks.
Another problem with this method is that it can produce a pretty crude
product if some simple precautions are not followed. From checking out
typical samples of street meth, it seems basic precautions are routinely
ignored. I believe that the by-products in the garbage meth are
iodoephedrine, and the previously mentioned azirine. (See the previous
section concerning chloroephedrine.) If a careful fractional distillation
is done, these products can be removed. They can be avoided in the first
place if, when making hydroiodic acid from iodine and red phosphorus, the
acid is prepared first, and allowed to come to complete reaction for 20
minutes before adding the ephedrine to it. This will be a hassle for some,
because the obvious procedure to follow is to use the water extract of the
ephedrine pills to make HI in. The way around the roadblock here is to just
boil off some more of the water from the ephedrine pill extract, and make
the acid mixture in fresh pure water. Since the production of HI from
iodine and red phosphorus gives off a good deal of heat, it is wise to
chill the mixture in ice, and slowly add the iodine crystals to the red
phosphorus-water mixture.
To do the reaction, a 1000 ml round bottom flask is filled with 150
grams of ephedrine hydrochloride (or PPA-HCL). The use of the sulfate salt
is unacceptable because HI reduces the sulfate ion, so this interferes with
the reaction. Also added to the flask are 40 grams of red phosphorus, and
340 ml of 47% hydroiodic acid. This same acid and red phosphorus mixture
can be prepared from adding 300 grams of iodine crystals to 50 grams of red
phosphorus in 300 ml of water. This should produce the strong hydroiodic
acid solution needed. Exactly how strong the acid needs to be, I can't say.
I can tell you that experiments have shown that one molar HI is ineffective
at reducing ephedrine to meth. The 47% acid mentioned above is a little
over 7 molar. I would think that so long as one is over 3 molar acid, the
reaction will work.
With the ingredients mixed together in the flask, a condenser is
attached to the flask, and the mixture is boiled for one day. This length
of time is needed for best yields and highest octane numbers on the
product. While it is cooking, the mixture is quite red and messy looking
from the red phosphorus floating around in it.
When one day of boiling under reflux is up, the flask is allowed to
cool, then it is diluted with an equal volume of water. Next, the red
phosphorus is filtered out. A series of doubled-up coffee filters will work
to get out all the red phosphorus, but real filter paper is better. The
filtered solution should look a golden color. A red color may indicate that
all the phosphorus is not out. If so, it is filtered again. The
filtered-out phosphorus can be saved for use in the next batch. If
filtering does not remove the red color, there may be iodine floating
around the solution. It can be removed by adding a few dashes of sodium
bisulfite or sodium thiosulfate.
The next step in processing the batch is to neutralize the acid. A
strong Iye solution is mixed up and added to the batch with shaking until
the batch is strongly basic. This brings the meth out as liquid free base
floating on top of the water. The strongly basic solution is shaken
vigorously to ensure that all the meth has been converted to the free base.
With free base meth now obtained, the next step, as usual, is to form
the crystalline hydrochloride salt of meth. To do this, a few hundred mls
of toluene is added to the batch, and the meth free base extracted out as
usual. If the chemist's cooking has been careful, the color of the toluene
extract will be clear to pale yellow. If this is the case, the product is
sufficiently pure to make nice white crystals just by bubbling dry HCL gas
through the toluene extract as described in Chapter 5. If the toluene
extract is darker colored, a distillation is called for to get pure meth
free base. The procedure for that is also described in Chapter 5. The yield
Cat is best made using chrome in the +6 oxidation state as the
oxidizer. I recall seeing an article in the narco swine's Journal of
Forensic Science bragging about how they worked out a method for making it
using permanganate, but that method gives an impure product in low yields.
Any of the common hexavalent chrome salts can be used as the oxidizer in
this reaction. This list includes chrome trioxide (CrO3), sodium or
potassium chromate (Na2CrO4), and sodium or potassium dichromate
of pure meth hydrochloride should be from 100 grams to 110 grams.
If gummy binders from the stimulant pills are carried over into the
reaction mixture, they produce a next-to-impossible-to-break emulsion of
meth, gum, toluene and water when the reaction is done and it is time to
extract out the meth. If this reaction is chosen as the production method,
one must be sure the gum has been thoroughly rinsed away with acetone from
the stimulant crystals. They should be long, white, and needle-like. If
this emulsion is encountered, the only way to break it is to first let the
emulsion sit in a sep funnel for a few hours. Water will slowly work its
way out and settle to the bottom where it can be drained away. The stubborn
residual emulsion should be transferred to a distilling flask, and the
toluene slowly distilled off through a fractionating column. This removes
water from the emulsion as the toluene-water azeotrope. It may be necessary
to add additionally toluene to the distilling flask to get all the water
removed. It sticks to the glass flask, and causes no further problem. Once
the emulsion is broken, distilling should be stopped. The toluene-meth
solution should be poured from the distilling flask, and the meth
precipitated as hydrochloride as per the usual dry HCl bubbling method.
--------------------------------------------------------------------------
Methcathinone
--------------------------------------------------------------------------
Kitchen Improvised Crank
The latest designer variant upon the amphetamine molecule to gain
popularity and publicity is methcathinone, commonly called "cat." This
substance is remarkably similar to the active ingredient found in the
leaves of the khat tree which the loyal drug warriors on the network news
blame for turning peace loving Somalis into murderous psychopaths. The
active ingredient in the khat leaves is cathinone, which has the same
structural relationship to methcathinone that amphetamine has to
methamphetamine. It is made by oxidizing ephedrine, while meth can be made
by reducing ephedrine.
The high produced by methcathinone is in many ways similar to
methamphetamine. For something so easily made and purified, it is actually
quite enjoyable. The main differences between the meth high and the
methcathinone high are length of action and body feel. With methcathinone,
one can expect to still get to sleep about 8 hours after a large dose. On
the down side, it definitely gives me the impression that the substance
raises the blood pressure quite markedly. This drug may not be safe for
people with weak hearts or blood vessels. Be warned!
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Old 10-26-2005, 10:29 AM   #33
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(Na2Cr2O3). All of these chemicals are very common. Chrome trioxide is used
in great quantities in chrome plating. The chromates are used in tanning
and leather making.
To make methcathinone, the chemist starts with the water extract of
ephedrine pills. The concentration of the reactants in this case is not
critically important, so it is most convenient to use the water extract of
the pills directly after filtering without any boiling away of the water.
See the section at the beginning of Chapter 15 on extracting ephedrine from
pills. Both ephedrine hydrochloride and sulfate can be used in this
reaction.
The water extract of 1000 ephedrine pills is placed into any convenient
glass container. A large measuring cup is probably best since it has a
pouring lip. Next, 75 grams of any of the above mentioned +6 chrome
compounds are added. They dissolve quite easily to form a reddish or orange
colored solution. Finally, concentrated sulfuric acid is added. If CrO3 is
being used, 21 ml is enough for the job. If one of the chromates is being
used, 42 ml is called for. These ingredients are thoroughly mixed together,
and allowed to sit for several hours with occasional stirring.
After several hours have passed, lye solution is added to the batch
until it is strongly basic. Very strong stirring accompanies this process
to ensure that the cat is converted to the free base. Next, the batch is
poured into a sep funnel, and a couple hundred mls of toluene is added.
Vigorous shaking, as usual, extracts the cat into the toluene layer. It
should be clear to pale yellow in color. The water layer should be orange
mixed with green. The green may settle out as a heavy sludge. The water
layer is thrown away, and the toluene layer containing the cat is washed
once with water, then poured into a beaker. Dry HCl gas is passed through
the toluene as described in Chapter 5 to get white crystals of cat. The
yield is between 15 and 20 grams. This reaction is scaled up quite easily.
--------------------------------------------------------------------------
MDA, XTC, and Other Psychedelic Amphetamines
--------------------------------------------------------------------------
The psychedelic amphetamines are a fascinating and largely ignored
group of drugs. They all have the basic amphetamine carbon skeleton
structure, but show effects that are more akin to LSD than to the amphetamines. The LSD-like effect is due to the presence of a variety of
"add ons" to the benzene ring of the basic amphetamine structure.
Generally, these "add ons" are ether groupings on the 3, 4, or 5 positions
on the benzene ring. Because of these "add ons" one can consider these
compounds more closely related to mescaline than to amphetamine. Consider
the mescaline molecule pictured on page 176.
Mescaline should by all rights be considered an amphetamine derivative.
It has the basic phenethylamine structure of the amphetamines with methyl
ether groupings on the benzene ring at the 3,4,5 positions. To be a true
amphetamine, it would only need its side chain extended by one carbon,
putting the nitrogen atom in the central, isopropyl position. Such a
compound does in fact exist. It is called trimethoxyamphetamine, or TMA for
short. Its effect are very similar to mescaline in much lower dosage levels
than the % gram required for pure mescaline. Its chemical cousin, TMA-2
(2,4,5 trimethoxyamphetamine) has similar awe inspiring characteristics.
The most popular and, in my opinion, the best of the psychedelic
amphetamines is the MDA family. This family consists of MDA, and its
methamphetamine analog, XTC, or Ecstasy, or
MDMA.MDA(3,4-methylenedioxyamphetamine) gives by far the best high of this
group. Its effects can best be described as being sort of like LSD without
the extreme excited state caused by that substance. It was popularly known
as "the love drug" because of the calm state of empathy so characteristic
of its effect. It could also be a powerful aphrodisiac under the right
circumstances.
This substance gradually disappeared during the early 80s due to an
effective crimping upon the chemicals needed for its easiest manufacture.
This crimping, and the drug laws in effect at the time, gave rise to a
bastard offspring of MDA. This substance was XTC, or MDMA, the so called
Ecstasy of the drug trade. This material was a designer variant of MDA, and
so was legal. The chemicals needed to make it could be obtained without
fear of a bust. It also lacked the best qualities of its parent. While the
addition of a methyl group of the nitrogen of the amphetamine molecule
accentuates its power and fine effect, the addition of a methyl group to
the MDA molecule merely served to make it legal. As fate would have it, the
hoopla surrounding the subsequent outlawing of this bastard child served to
make it a more desired substance than MDA. This is typical of black-market,
prohibition-driven demand.
To understand the various routes which can be followed to make these
substances, note the structures of MDA and MDMA shown below:
To make these substances, and the rest of the psychedelic amphetamines
for that matter, the manufacturer has a choice of two starting materials.
He can use the appropriately substituted benzaldehyde, which in the case of
MDA or MDMA is piperonal (heliotropin), or he can use the correspondingly
substituted allylbenzene, which in this case is safrole.
Piperonal was the favored starting material for making MDA, as were the
other substituted benzaldehydes for making other psychedelic amphetamines.
The supply of these raw materials was effectively shut off. Piperonal does
find legitimate use in making perfumes, but considerable determination is
needed to divert significant amounts of the stuff into clandestine
operations.
Once obtained, these substituted benzaldehydes could be converted into
amphetamines by an interesting variant of the Knoevenagel reaction as
described in Chapter 9. They could be reacted in a mixture of nitroethane
and ammonium acetate to form the appropriately substituted
1-phenyl-2-nitropropene. This nitropropene could then be reduced to the
amphetamine by using lithium aluminum hydride, or palladium black on
charcoal in a hydrogenation bomb. This pathway was further crimped upon by
the narco swine by watching for purchases of nitroethane and ammonium
acetate in combination. For all practical purposes, this pathway can be
considered dead.
This left safrole, and the other substituted allylbenzenes, as starting
materials for psychedelic amphetamine manufacture. This route had the
advantage of having a raw material source that was nearly impossible to
shut down. For instance, sassafras oil consists of 80-90% safrole. One
merely has to distill the oil under a vacuum to get very pure safrole.
Similarly, other psychedelic amphetamines can be made from the
allylbenzenes naturally occurring in various plant oils. For instance,
calamus oil contains a large proportion of B-asarone the starting material
for TMA-2. Nutmeg contains a mixture of myristicin (potential MMDA) and
elemicin (potential TMA). These oils are all available from herbal supply
shops and dealers in the occult. Even without this source, the oils can be
easily obtained from the plants.
The reason why the markets have not been flooded with psychedelic
amphetamines via the allylbenzene source is because the only method for
converting them into amphetamines that was widely known is very cumbersome.
For instance, the only method for making MDA from safrole that was listed
in Psychedelic Chemistry was the old tedious route. This route called for
first converting safrole to isosafrole by the action of alcoholic KOH at
243C for 3 minutes. This isosafrole could then be converted to MDA
phenylacetone by a very messy and inefficient method using hydrogen
peroxide in a solution of acetone and formic acid. This step is so poor
that it rendered the whole route unworkable. Finally, the MDA phenylacetone
could be made into MDA by one of several methods. It is interesting that
Michael Valentine Smith copied the printing error that appeared in Chem
Abstracts concerning this last step into his book.
Luckily, the relentless advance of chemical science has lifted this
roadblock. The same method which was earlier described for converting
allylbenzene into phenylacetone is equally useful for converting
substituted allylbenzenes directly into the corresponding substituted
phenylacetones. The yield in these reactions is nearly as good as for
phenylacetone itself, and the procedure is just as easy.
The first problem which confronts the chemist in the process of turning
sassafras oil into MDA or MDMA is the need to obtain pure safrole from it.
In spite of the fact that crude sassafras oil consists of 80-90% safrole,
depending on its source, it is a good bet that the impurities will lower
the yield of the desired product. The axiom "garbage in, garbage out" was
custom made for organic chemistry reactions. It is simplicity itself to
turn crude sassafras oil into pure safrole, and well worth the effort of
underground chemists bent on MDA production.
Sassafras oil is an orange colored liquid with a smell just like
licorice. It is a complex mixture of substances which is easily purified by
distilling. To obtain pure safrole from sassafras oil, the glassware is set
up as shown in Figure 5 in Chapter 3. The distilling flask is filled about
2/3 full of sassafras oil, along with a few boiling chips, and then vacuum
is applied to the system. A little bit of boiling results due to water in
the oil, but heat from the buffet range is required to get things moving.
Water along with eugenol and related substances distill at the lower
temperatures. Then comes the safrole fraction. The safrole fraction is
easily spotted because the "oil mixed with water" appearance of the watery
forerun is replaced with a clear, homogeneous run of safrole. When the
safrole begins distilling, the collecting flask is replaced with a clean
new one to receive it. The chemist is mindful that the safrole product is
80-90% of the total volume of the sassafras oil. Under a vacuum, it boils
at temperatures similar to phenylacetone and methamphetamine. When all the
safrole has distilled, a small residue of dark orange colored liquid
remains in the distilling flask. The distilled safrole is watery in
appearance, and smells like licorice.
With a liberal supply of safrole obtained by distilling sassafras oil,
work can then commence on converting it into 3,4
methylenedioxyphenylacetone. This is done in exactly the same manner as
described in Chapter 10. As was the case in that chapter, the chemist has
the choice of the palladium-wasteful method, and the palladium-conserving
method. As was the case in the earlier chapter, the yield of product is
about 10% higher using the palladium-wasteful method. The yield is about
93% for the wasteful method, versus about 83% for the conserving method.
The sole difference in the safrole conversion reaction is that in this
case, palladium bromide is used instead of the palladium chloride used to
convert allylbenzene. Since palladium bromide has a higher molecular weight
than palladium chloride, the amount of palladium salt used in this case is
increased by a factor of 1.5.
The methylenedioxyphenylacetone obtained from this reaction can be used
in a crude state by boiling off the solvents from it under a vacuum, or it
can be distilled under a vacuum to yield pure material. The boiling point
of this phenylacetone is around 180C at a pressure of 15 torn The color of
the distilled material is clear to pale yellow.
With the methylenedioxyphenylacetone obtained in this manner, the
chemist proceeds to make it into XTC by one of the methods used to turn
phenylacetone into meth. Of all the methods to choose from, the most
favored one would have to be reductive alkylation using the bomb and
platinum catalyst. The free base is converted into crystalline
hydrochloride salt in exactly the same manner as for making meth crystals.
It is interesting to note here that XTC crystals will grow in the form of
little strings in the ether solution as the HCl gas is bubbled through it.
Once filtered and dried, it bears a remarkable resemblance to meth
crystals. It generally has a faint odor which reminds one of licorice.
To make MDA from the methylenedioxyphenylacetone, one has two good
choices. Choice number one is to use the reductive amination method without
the bomb using activated aluminum as the reducer. In this case, 28% ammonia
solution in water (ammonium hydroxide, NH4OH) is used instead of 40%
methylamine in water. The amount of ammonia solution used is doubled over
the amount of methylamine solution used. Other than that, the reaction
proceeds just as in the case for meth and gives a yield around 40%. The
next best method is to use the bomb with Raney nickel catalyst and ammonia.
This gives a yield around 80% if plenty of Raney nickel is used. The
drawback to this method is the need for a shaker device for the bomb, and
also a heater. The use of platinum as the catalyst in the bomb works great
when making MDMA, but gives lousy results when making MDA. There may be a
way around this, however, for serious experimenters. It has been found in
experiments with phenylacetone that a mixture of ammonia and ammonium
chloride produces good yields of amphetamine (50%) when used in a bomb with
platinum catalyst. Methylenedioxyphenylacetone is quite likely to behave
similarly.
To use this variation, the following materials are placed in the 1.5
liter champagne bottle hydrogenation device: .5 gram platinum in 20 ml
distilled water. If this platinum is in the form of PtO2 instead of the
reduced platinum metal catalyst obtained with borohydride, the experimenter
must now reduce the platinum by pressurizing the bottle with hydrogen and
stirring for about an hour. Next 100 ml of methylenedioxyphenylacetone is
added along with 40 grams NH4Cl, 500 ml methyl alcohol saturated with
ammonia gas, and 50 ml NH4OH. The bottle is then set up as seen in Figure
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Old 10-26-2005, 10:30 AM   #34
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17. and the hydrogenation is done as described in that section.
When the reaction is over, the contents of the flask are filtered to
remove the platinum metal for reuse. Some crystals of NH4Cl are also
filtered out; they are rinsed down with some water to remove them.
Next the filtered batch is poured into a 1000 ml round bottom flask, a
few boiling chips are added, and the glassware is set up for refluxing.
Plastic tubing is attached to the top of the condenser and led outside. The
mixture is boiled under reflux for one hour to force out the excess
ammonia.
Next, the solution is allowed to cool, and made acid to congo red
(about pH 3) with hydrochloric acid. Now the glassware is set up as shown
in Figure 3, and the solution is evaporated to about one half its original
volume under vacuum. A fair amount of crystalline material forms during the
acidification and vacuum evaporation.
Next, 400 ml of water is added to the solution, and then it is
extracted with about 100 ml of toluene. The toluene layer is thrown away
because it contains garbage. The batch is now made strongly basic by adding
lye water to it. It should be remembered here that it is very important to
shake the batch well once it has been basified to make sure that the MDA
hydrochloride gets neutralized. Finally, the MDA is extracted out with a
few hundred ml of toluene, and distilled under vacuum. The boiling point is
about 170C under aspirator vacuum. The yield is about 50 ml.
The other good choice of a method for converting
methylenedioxyphenylacetone into MDA is the Leuckardt reaction. In this
case, formamide is used instead of N-methylformamide. The formamide is of
the 99% pure grade. 98% formamide is good for nothing except making the
dreaded red tar. Good luck in finding 99% formamide these days. This
reaction is done in exactly the same manner as the reaction with
N-methylformamide, except that the reaction temperature is 160 to 185C,
raised over the course of 24 hours. The yields are excellent. Processing is
done as in the case of meth. The formamide is destroyed by boiling with lye
solution. In this case the ammonia gas produced is just led away in tubing.
The formyl amide is then separated and hydrolyzed with hydrochloric acid
solution.
Another possible route to MDA and other psychedelic amphetamines is the
Ritter reaction. It was encountered earlier in Chapter 14. Since safrole
and many other plant oil precursors to the psychedelic amphetamines, such
as myristicin, are allylbenzenes, this reaction will work for them as well.
with some modifications to the process.
The first modification is that alcoholic KOH is used to hydrolyze the
amide instead of HCl solution. Boiling the amide with about 5 to 10 volumes
of 10% KOH solution in 190 proof vodka gives better results than
hydrochloric acid. Less tar and other by-products will result. 190 proof
vodka and rectified spirit is used, not absolute alcohol. Refluxing for
about 5 hours does the job.
To process the product, the underground chemist first boils away most
of the alcohol under a vacuum, then adds water to dissolve the KOH, and
extracts out the MDA using benzene or toluene. He distills and crystallizes
as usual.
XTC can be obtained from MDA by using the method cited in the Woodruff
article referred to in Chapter 14.
The yield and purity of the MDA obtained from the Ritter reaction is
somewhat less than with the two step method using palladium salts and
nitrites. This disadvantage must be weighted against the fact that the
Ritter reaction uses very simple, cheap, and easily available chemicals.
Not all psychedelic amphetamines can be produced in this manner. For
instance, B-asarone, the precursor of TMA-2, is a 2propenyl-benzene, rather
than an allylbenzene. The breakthrough method will fail in this case, and
the Ritter reaction will yield an isoquinoline. To convert
2-propenylbenzenes directly into amphetamines, a very risky reaction using
is used. See Recreational Drugs by Professor Buzz for details.
For the same reason of relative molecular weight, if safrole is used in
either the phenylacetone from allylbenzene method or in the Ritter
reaction, the amount of safrole used is greater by a factor of about 1.35
as compared to allylbenzene.
The recommended dosage of MDA or XTC is about a tenth of a gram of Pure
material.
References
Psychedelics Encyclopedia by Peter Stafford.
--------------------------------------------------------------------------
Ice
--------------------------------------------------------------------------
At the time of the writing of the second edition, the latest drug craze
was the smokable form of methamphetamine called "ice." This material
consists of large clear crystals of methamphetamine hydrochloride rather
than the snowlike microcrystals produced by the methods described in this
book.
I am not going to endorse or encourage the foolhardy practice of
smoking meth. Seeing firsthand what this stuff does to rubber stoppers,
razor blades, and corks, I can only imagine what it does to lung tissue.
However, since the godless importers of this material have already made a
market for it, it is only right that I help American technology catch up.
I have never made nor used "ice" as such, but I know quite well how to
obtain large clear rocklike crystals of meth. There are two routes which
can be followed. The first is to simply melt the pure meth crystals and
then allow them to slowly cool into a solid mass. This is a piss poor
choice because the heat is likely to discolor even very pure meth melted
under a nitrogen atmosphere blanket. The accompanying "off" smell and god
knows what breakdown products make this a method that only hacks would use.
A much better method is to take the pure meth crystals, and add just
enough absolute alcohol to them to dissolve them. Gentle heating, swirling,
and the use of warm alcohol keeps the volume of alcohol used to a minimum.
The beaker holding the dissolved meth is then put into a dessicator to
prevent the alcohol from soaking up water from the air. If the desiccator
has a portal for the attachment of vacuum, this is ideal. Then a vacuum
amounting to 1/2 normal pressure is applied, and the solution slowly cools
and evaporates its alcohol solvent. The result is a large rocklike mass of
meth which can then be chipped off of the beaker.
--------------------------------------------------------------------------
Calibrating The Vacuum
--------------------------------------------------------------------------
Before he starts doing the vacuum distillations described in this book,
the underground chemist wants to know what kind of vacuum he is able to
produce inside his glassware. This is important because the temperature at
which a substance distills under vacuum depends directly on how strong the
vacuum is. The distillation temperatures given in this book assume a vacuum
of about 20 torr for an aspirator and about 5 torr for a vacuum pump. This
chapter describes an easy method by which the chemist finds out just how
strong his vacuum is. Once he knows how good his vacuum is, he adjusts the
temperatures of his distillations accordingly. The better the vacuum, the
lower the temperature at which the substance will distill. He keeps in mind
that an aspirator will get a better vacuum in winter because the water
flowing through it is colder in that season. The vacuum obtained with a
vacuum pump may get poorer over time because solvents from the chemicals he
is distilling, such as benzene, may dissolve in the pump's oil. If this
happens, he changes the oil.
To begin, the chemist sets up the glassware for fractional distillation
as shown in Figure 5 in Chapter 3. He uses a 500 ml round bottom flask for
the distilling flask, and a 250 ml flask as the collecting flask. He uses
the shorter condenser, and puts 3 boiling chips in the distilling flask
along with 200 ml of lukewarm water. He lightly greases all the ground
glass joints. (This is always done when distilling, because the silicone
grease keeps the pieces from getting stuck together, and seals the joint so
that it doesn't leak under the vacuum).
He turns on the vacuum full force and attaches the vacuum hose to the
vacuum nipple of the vacuum adapter. The water in the distilling flask
should begin boiling immediately. As the water boils away, the temperature
shown on the thermometer steadily drops. Finally, the water gets cold
enough that it no longer boils. He notes the temperature reading when this
happens, or, better yet, disconnects the vacuum and takes apart the
glassware and takes the temperature of the water in the distilling flask.
Using a graph such as the one above, he reads off the vacuum that goes with
the boiling temperature.
If his vacuum is bad, the water will not boil. In that case, he checks
to make sure that all the joints are tight, and that the stopper in the
claisen adapter fractionating column is not leaking. He also makes sure
that his vacuum hose is not collapsed. If, after this, the water still
doesn't boil, he has to heat the water. He turns on the buffet range at low
heat while continuing the vacuum. In a while the water begins boiling. He
checks the temperature reading on the thermometer while it is boiling, and
notes the temperature. From the graph he reads off the vacuum that goes
with that boiling point.
His vacuum should be 50 torr or lower to be able to make
methamphetamine. If his vacuum reading is more than 50 torr, he gets a new
aspirator or changes the oil in the vacuum pump.
The chemist can use this information to adjust the temperature at which
he collects his distilled product. The boiling temperature of phenylacetone
is about 105C at 13 torr, and about 115C at 20 torn The boiling
temperature of N-methylformamide is about 107C at 20 torn The boiling
temperature of methamphetamine is about the same as phenylacetone.
Phenylacetone and methamphetamine should be collected over a 20-degree
range centered on their true boiling points. This makes sure that the
chemist gets all of it. The purification scheme he goes through before
distilling removes all the impurities with boiling points close to that of
his product.--------------------------------------------------------------------------
Transcriber's Notes:
I have omitted many of the pictures in the book, I want you to see this as
a reason to buy the real book instead of this ASCII version. This is a part
of my shareware book concept; If you want to have the whole book, then go
buy it. You can order it directly from Loompanics Unlimited, PO Box 1197,
Port Townsend, WA 98368, USA. A fourth edition is on its way, Fester says.
-------------------------------------------------------------------------
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Old 10-31-2005, 02:41 AM   #35
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Gimme a break!

you took something that's pretty simple and made it sound complicated as hell!

And FYI:
The lithium- ammonia reduction is not "new" -it's old as hell.
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Old 10-31-2005, 02:26 PM   #36
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i didnt say it was new, only the best.with start to finish time just over an hour and 90-95% pure.and the book isnt that hard to follow
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Old 11-01-2005, 12:44 PM   #37
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lol did you ask the author if you could write this out? or are you the author?
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Old 11-01-2005, 01:45 PM   #38
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Anyone can look up patents.
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Old 11-01-2005, 11:39 PM   #39
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this is the shareware virsion -so no pics-and its only 3rd eddition
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Old 11-02-2005, 10:08 PM   #40
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congratulations for contributing to the increase of the allready overpopulated tweaker population.
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