LSD-The One-Pot Shot

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    LSD Directly From The
    Lysergic Amides
    — The One-Pot Shot

    When the lysergic amides have been extracted in pure form from
    the crop, work should begin without delay to convert it to LSD.
    Diligence in this matter is very important because possession of the
    extracted amides is strong evidence of intent to manufacture LSD.
    Further, mere possession of lysergic acid or ergine is prohibited as
    they are federal "controlled substances." The goal must be to get the
    hot potato out of one's hands and convert it to cash as fast as possible.
    There are several possible methods to follow in the conversion of
    the lysergic amides to LSD. The first two presented in this book are
    excellent, and highly recommended. The third one is OK. Beyond
    that, we are talking last resort. In all cases, the overriding factor which
    must take precedence is ease of availability of the required chemicals. A
    bottle of trifluoroacetic anhydride in hand beats homemade
    anhydrous hydrazine in the bush.

    The first LSD manufacture method presented here is what I like to
    call "the one-pot shot." It can be found in US patent 3,239,530 and
    US patent 3,085,092, both granted to Albert Hofmann. This method
    uses anhydrous hydrazine to cleave the ergot amides to produce
    lysergic acid hydrazide. The hydrazide is then isolated by extraction,
    and reacted with acetylacetone (2,4-pentanedione) to form a pyrazole
    intermediate, which is then reacted with diethylamine to form LSD.
    This method at first glance seems complicated, but the actual
    manipulations involved here are less challenging than proceeding
    through lysergic acid. Further, the yields are higher with this method
    than those proceeding through lysergic acid, and there is less
    formation of the inactive iso-LSD than with other methods. Iso-LSD is
    not a complete loss since it can be converted to the active LSD, but it is
    best to avoid its formation in the first place.

    This method has a serious drawback. Anhydrous hydrazine is not
    available off the shelf at your local hardware store, and attempts to
    procure it through normal channels are likely to catch the attention of
    those shit-eating dogs at the DBA. I include in this chapter directions for
    making your own anhydrous hydrazine, but be warned here that
    failure to use a nitrogen atmosphere during the distillation of
    anhydrous hydrazine will likely lead to an explosion. On that cheery
    note, let's begin!

    Step One:
    Conversion of Ergot Amides
    to Lysergic Acid Hvdrazide

    The reaction above is illustrated for ergotamine, but the process is
    just as valid when a mixture of amides is used as extracted from the
    crop. Further, the crop amides have been left in the freebase form, so
    the procedure given in example 5 in US patent 3,239,530 is used. This is
    superior to trying to make a hydrochloride salt of the amides, as
    suggested in example 1, because this would expose the active
    ingredients to loss and destruction during the unnecessary handling.
    There are three main precautions to be followed while executing
    this procedure. Water must be rigorously excluded from the reaction
    mixture, as hydrazine hydrate will react with the amides to form
    racemic lysergic acid hydrazide rather than our desired product. To
    ensure the exclusion of water from the reaction, the glassware should be
    baked in an electric oven prior to use, and be allowed to cool off in a
    dessicator. A drying tube should be attached to the top of the
    condenser used, to prevent humidity in the air from getting in the mix.
    Naturally, the hydrazine used had better be anhydrous.
    Another danger to success is exposure to light. Work should be
    done under a dim red darkroom bulb. The flask containing the
    reaction mixture should be wrapped in aluminum foil to exclude light.
    Procedures such as extractions and filtering should be done as rapidly as
    possible without causing spills.

    Finally, this reaction should be done under a nitrogen atmosphere,
    as hot hydrazine and oxygen do not get along too well.
    In a 500 ml round-bottom flask place a magnetic stirring bar, 10
    grams of the ergot amide mixture (dried in a vacuum dessicator to
    ensure its freedom from water), 50 ml of anhydrous hydrazine, and 10 ml
    of glacial acetic acid. A condenser equipped with a drying tube is then
    attached to the flask, and the flask wrapped in a single layer of
    aluminum foil. The flask is then lowered into a glass dish containing
    cooking oil heated to 140° C on a magnetic-stirrer hot-plate. When the
    flask goes into the oil, the heat should be backed off on the hot-plate so
    that both oil and flask meet each other in the middle at 120° C.
    Monitor the warming of the contents of the flask by occasional
    insertion of a thermometer. Stir at moderate speed. In about 10
    minutes, the desired temperature range is reached, and some gentle
    boiling begins. Maintain the temperature of the oil bath at 120-125° C,
    and heat the batch for 30 minutes.

    When 30 minutes heating at 120° C is complete, add 200 ml
    water to the batch, increase the oil temperature to 140° C, and rig the
    glassware for simple distillation. Distill off between 200 to 250 ml
    water, hydrazine hydrate and acetic acid mixture. Then remove the
    flask from the heated oil, and allow it to cool. Use of an aspirator
    vacuum to assist the distillation is highly recommended.

    When the flask has cooled, add 100 ml of decimolar tartaric-acid
    solution (1.5 grams tartaric acid in 100 ml water) to the flask, and 100
    ml ether. Stopper the flask, and shake vigorously for a few minutes,
    with frequent breaks to vent off built-up pressure from the flask. If the
    stirring bar bangs too violently in the flask, remove it with a magnet
    rather than break the flask.

    Pour the contents of the flask into a 250 ml sep funnel, and drain
    the lower layer (water solution of lysergic acid hydrazide tartarate)
    into a 250 ml Erlenmeyer flask wrapped in foil. To the ether layer still in
    the sep funnel, add 50 ml fresh decimolar tartaric-acid solution, and
    shake. Examine the water layer for the presence of lysergic acid
    hydrazide with a black light. If there is a significant amount, add this
    also to the Erlenmeyer flask.

    Place the magnetic stirring bar in the Erlenmeyer flask, and stir it
    moderately. Monitor the pH of the solution with a properly calibrated
    pH meter, and slowly add .5M (20 grams per liter) sodium hydroxide
    solution until the pH has risen to the range of 8-8.5. Higher pH will
    cause racemization. The freebase is then extracted from the water
    solution with chloroform. Two extractions with 100 ml of chloroform
    should complete the extraction, but check a third extraction with the
    black light to ensure that most all of the product lysergic acid
    hydrazide has been extracted.

    The chloroform extracts should be evaporated under a vacuum in a
    500 ml flask to yield the product. This is best done by rigging the 500
    ml flask for simple distillation, and applying an aspirator vacuum to
    remove the chloroform. Assume that the yield from this procedure will
    be about 5 grams of lysergic acid hydrazide if ergot was the crop used.
    Assume that the yield will be about 7.5 grams if seeds were used.
    The difference here is due to the fact that in ergot, the amides
    are largely composed of substances in which the portion lopped off is
    about as large as the lysergic acid molecule. Seeds tend to be more
    conservative as to their building upon the lysergic molecule. A careful
    weighing on a sensitive scale comparing the weight of the flask before
    and after would give a more exact number.
    Both of these choices are really very poor, because lysergic acid
    hydrazide, unlike most other lysergic compounds, crystallizes very
    well with negligible loss of product. At the hydrazide stage of LSD
    manufacture, one has a perfect opportunity to get an exceedingly pure
    product, freed from clavine alkaloids and other garbage compounds
    carried in from the extraction of the complex plant material.
    I refer the reader to US patent 2,090,429 issued to Albert
    Hofmann and Arthur Stoll, the dynamic duo of lysergic chemistry,
    dealing with lysergic acid hydrazide. In this patent, they describe in a
    rather excited state how they were able to produce pure lysergic acid
    hydrazide from tank scrapings that were otherwise impure junk.
    Lysergic acid hydrazide has the following properties: it dissolves
    easily in acid, but is very difficultly soluble in water, ether, benzene
    and chloroform. In hot absolute ethanol it is slightly soluble, and is
    crystallizable in this solvent to yield "beautiful, compact, clear, on sixsided
    cut-crystal plates that melt with decomposition at 235-240° C."
    This is obviously the way to go. The hydrazide should be
    recrystallized from absolute ethanol, and then dried under a vacuum to
    remove residual alcohol clinging to the crystals. About 300 ml of hot
    ethanol is required to dissolve each gram of lysergic acid hydrazide
    during the crystallization. Upon cooling, a first crop of pure lysergic
    acid hydrazide is obtained. Then, by boiling away half of the mother
    liquor and cooling, an additional crop is obtained. This process can be
    continued as long as the crystals obtained look nice.

    Step Two: Lysergic Acid
    Pyrazole

    In this reaction, one mole of lysergic acid hydrazide is dissolved in
    an inert, water-miscible solvent like ethanol. Then an excess of 1-molar
    hydrochloric acid is added to form a salt with the lysergic acid
    hydrazide. To this mixture is then added two moles of acetylacetone
    (2,4-pentanedione), which forms the desired pyrazole. This reaction is
    not nearly as touchy as the formation of the hydrazide. The presence of
    traces of moisture from the air poses no problem. 2,4-pentanedione finds
    use in analytical chemistry as a chelating agent for transition metals,
    and as such should be available without raising too many red flags.
    Synthesis of this compound is not hard, and directions for doing so are
    found in US Patents 2,737,528 and 2,834,811.

    To do the reaction, the flask containing the 5 grams of hydrazide is
    wrapped in a single layer of foil to exclude light. Then a magnetic
    stirring bar is added, along with 18 ml of ethanol, 18 ml water, 20 ml 1-
    molar HC1 (made by adding one part 37% HC1 to 11 parts water) and
    this mixture is stirred for a few minutes. Then 3.5 grams (3.5 ml) of
    2,4-pentanedione is added at room temperature, and the stirring
    continued for an hour or so.

    The product is recovered from solution by the slow addition with
    stirring of 20 ml 1-molar NaOH (40 grams per liter). This
    neutralization throws the pyrazole out of solution as a solid. The solid is
    collected by filtration through a Buchner funnel, and rinsed off with
    some water. The crystals are then dried under a vacuum, preferably
    with the temperature elevated to 60° C. Further purification can be
    done by crystallization. If so desired, dissolve the crystals in
    chloroform, then add 8-10 volumes of ether to precipitate the product. I
    do not feel this is necessary if the hydrazide used was reasonably
    pure, since all the reagents used in the last step are soluble in water.
    The water rinse should have carried them away. Further, alcohol and
    2,4-pentanedione are volatile, and would be removed in the vacuum
    drying.

    Step Three:
    LSD

    This simple and easy reaction is done as follows: In a flask
    wrapped in a single layer of foil are placed 1 gram lysergic acid
    pyrazole, and 30 ml diethylamine. Diethylamine is a definite "do not
    purchase" item. Easy directions for its synthesis are given in this
    chapter. The two ingredients are swirled until mixed, then allowed to
    stand at room temperature for about a day.

    The excess diethylamine is then distilled off, and saved for use in
    future batches. Dimethylpyrazole is a high-boiling-point substance,
    and easily separated from diethylamine. When most of the
    diethylamine has been distilled off, a vacuum is applied, and the
    residue is evaporated to dryness. The evaporation is completed by
    warming the flask in boiling water for a few minutes with continued
    application of vacuum. The residue is almost pure LSD.

    Purification and Storage

    At this point, the process has yielded LSD freebase. In this state,
    the substance is quite unstable and not suitable for storage. A
    judgment as to the purity of the product is therefore needed in quick
    order, because which method of further processing to use is dependent
    upon the purity of the product. If there is reason to believe that a
    significant amount of iso-LSD is mixed in with the product, the
    following chromatographic separation is called for. The iso-LSD can
    then be recovered and converted to the active LSD, which greatly
    increases the value of the product. Iso-LSD can be expected to be
    formed using the process in this chapter if the additions of sodium
    hydroxide were not sufficiently slow, and local areas of high pH
    developed in the solution. Using methods in other chapters proceeding
    through lysergic acid, a large amount of the iso product can be
    expected if lysergic acid was made by use of hydrazine hydrate or HOH.
    Also, some of the natural alkaloids are of the iso form and yield iso-
    LSD. The procedure for acid production using trifluoroacetic anhydride
    will always make a lot of the iso product. The best procedure I can
    recommend is: whatever method has been used, check the product
    through chromatography for the presence of the iso-LSD. The following
    procedure is taken from US patent 2,736,728.

    3.5 grams of LSD freebase is dissolved in 160 ml of a 3-1 mixture of
    benzene and chloroform (120 ml benzene, 40 ml chloroform).
    Next, a chromatography column is constructed from a burette. It must
    hold about 240 grams of basic alumina (not acidic alumina), so a 100
    ml burette is called for. A wad of cotton and filter paper is stuffed
    down the burette against the stopcock to keep the particles of alumina
    from flowing out. The 240 grams of basic alumina are then poured
    into the burette with tapping to assure it is well packed. The alumina
    should then be wetted with some 3-1 benzene-chloroform. Now the 160 ml of benzene-chloroform containing the LSD is run
    slowly into the burette, followed by more benzene-chloroform to
    develop the chromatogram. As the mixture flows downward through
    the alumina, two zones that fluoresce blue can be spotted by
    illumination with a black light. The faster-moving zone contains LSD,
    while the slower-moving zone is iso-LSD.

    When the zone containing LSD reaches the spigot of the burette, it
    should be collected in a separate flask. About 3000 ml of the 3-1
    benzene-chloroform is required to get the LSD moved down the
    chromatography column, and finally eluted.

    The iso-LSD is then flushed from the column by switching the
    solvent being fed into the top of the column to chloroform. This
    material is collected in a separate flask, and the solvent removed
    under a vacuum. The residue is iso-LSD, and should be stored in the
    freezer until conversion to LSD is undertaken. Directions for this are
    also given in this chapter.

    For the fraction containing the LSD, conversion to LSD tartrate
    must be done to make it water soluble, improve its keeping
    characteristics, and to allow crystallization. Tartaric acid has the
    ability to react with two molecules of LSD. Use, then, of a 50% excess of
    tartaric acid dictates the use of about 1 gram of tartaric acid to 3
    grams of LSD. The three grams of LSD would be expected from a
    well-done batch out of a total 3.5 LSD/iso-LSD mix.
    The crystalline tartrate is made by dissolving one gram of tartaric
    acid in a few mis of methanol, and adding this acid solution to the
    benzene-chloroform elute from the chromatography column.
    Evaporation of the solvent to a low volume under a vacuum gives
    crystalline LSD tartrate. Crystals are often difficult to obtain. Instead,
    an oil may result due to the presence of impurities. This is not cause
    for alarm; the oil is still likely 90%+ pure. It should be bottled up in
    dark glass, preferably under a nitrogen atmosphere, and kept in a
    freezer until moved.

    If chromatography reveals that one's chosen cooking method
    produces little of the iso products, then the production of the tartrate
    salt and crystallization is simplified. The residue obtained at the end
    of the batch is dissolved in a minimum amount of methanol. To this is
    then added tartaric acid. The same amount is added as above: one gram
    tartaric acid to three grams LSD. Next, ether is slowly added with
    vigorous stirring until a precipitate begins to form. The stoppered flask is
    then put in the freezer overnight to complete the precipitation. After
    filtering or centrifuging to isolate the product, it is transferred to a dark
    bottle, preferably under nitrogen, and kept in the freezer until moved.
    LSD from iso-LSD.

    Two variations on this procedure will be presented here. The first is
    the method of Smith and Timmis from The Journal of the
    Chemistry Society Volume 139, H pages 1168-1169 (1936). The other is
    found in US patent 2,736,728. Both use the action of a strong
    hydroxide solution to convert iso material into a mixture that contains
    active and iso material. At equilibrium, the mixture contains about 2/3
    active material and 1/3 iso material. These substances are separated by
    chromatography, and the iso material saved to be added to the batch
    the next time isomerization is done. In this way, eventually all of the
    product becomes active material.

    Method One

    The iso-LSD as eluted from the chromatography column is first
    evaporated under a vacuum to remove the solvent. The residue is then
    dissolved in 1-molar alcoholic KOH, and boiled under reflux,
    preferably with a nitrogen atmosphere, for 30 minutes.
    The mixture is next cooled and diluted with 3 volumes of water. It is
    next acidified with HC1, then made alkaline again with sodium
    carbonate. The product is now extracted from solution with ether or
    chloroform. After removal of the solvent, the product can be chromatographed as previously described.

    Method Two

    The iso-LSD as eluted from the chromatography is first
    evaporated under a vacuum to remove the solvent. The residue is
    dissolved in the minimum amount of alcohol, and then one half
    volume of 4-molar KOH in 100 proof vodka is added. The mixture is
    allowed to sit at room temperature for a couple of hours, then the
    alkali is neutralized by adding dry ice. The solvents are next removed
    under a vacuum, and the residue chromatographed as previously
    described.

    Preparation of Anhydrous Hydrazine

    Anhydrous hydrazine can be made from the easily available raw
    materials: bleach, ammonia, sulfuric acid and potassium hydroxide.
    This is not a task to be undertaken lightly, as there are dangers
    inherent in the process. Hydrazine will likely detonate during
    distillation if the distillation is not done in a nitrogen atmosphere.
    Also, hydrazine is a vicious poison prone to absorption through the
    skin or by inhalation of its vapors. It is very corrosive to living tissue,
    and its burning effects may be delayed. Hydrazine can also be
    assumed to be a carcinogen. All steps in its preparation must be done
    with proper ventilation, and protection of the body from spills.

    Step One: Hydrazine Sulfate

    2NH3
    + NaOCI ——> NH2 NH2 + H2O + NaCI NH2NH2
    + H2S04 ——> NH2 NH2 H2S 04

    Into a 3-quart-capacity glass baking dish (Pyrex) put 750 ml
    strong ammonia (28% NH3), 350 ml distilled water, 190 ml 10%
    gelatine solution, and 700 ml 12.5% bleach. This strength of bleach is
    available from pool supply companies and makers of cleaners. The
    5.25% strength Clorox will not do here. One must also be aware that
    traces of iron and copper have a very bad effect upon the yield, so do
    not dispense with the use of distilled water. The bleach is another
    possible source of iron. In checking out this reaction, the Pro
    Chemicals brand of bleach worked fine. I can't vouch for other
    brands. If all else fails, the bleach can be made from chlorine and
    NaOH in distilled water. (See Organic Syntheses Collective Volume 1,
    page 309.) The Pro Chemicals brand of bleach analyzed at 10 ppm iron
    by atomic absorption, and this amount did not interfere with the
    reaction. One must also check the bleach to make sure it is alkaline, as
    free chlorine prevents the formation of hydrazine.
    When the ingredients have been mixed in the baking dish, it is
    heated as rapidly as possible until it has been boiled down to one-third of
    its original volume. Being a wimp and boiling it down too slowly
    reduces the yield. Take not more than two hours.
    The dish is then removed from the heat, and allowed to cool.
    When the dish nears room temperature, it should be nestled in ice to
    chill thoroughly. The solution should then be filtered to remove
    suspended particles from the solution.

    The filtered solution is next put in a beaker, and nestled in ice
    mixed with salt until the temperature of the solution reaches 0° C.
    When that temperature is reached, 10 ml of concentrated sulfuric acid
    for each 100 ml of solution is slowly added with constant stirring. If
    the stirring is not strong, or if the filtering was poorly done, a product
    contaminated with brown particles results. If done well, hydrazine
    sulfate precipitates as white crystals. The mixture is allowed to stand in
    the cold for a few hours to complete the precipitation. The crystals are
    then filtered by suction, and the crystals rinsed off with cold
    alcohol. The yield is 25 to 30 grams of hydrazine sulfate.

    Step Two:
    Hydrazine Hydrate

    Mix 100 grams dry hydrazine sulfate with 100 grams powdered
    KOH and place the mixture into a copper and silver retort. Then add 15
    ml water, and distill off the hydrazine hydrate formed though a
    downward-inclined glass condenser. There is little need for heat to be
    applied at the beginning of the distillation because so much heat is
    generated in the reaction between the KOH and the sulfate. Later,
    strong heating is required to distill out the last of the hydrazine
    hydrate.

    This crude product contains water beyond the monohydration of
    hydrazine. It is purified by fractional distillation. Pure hydrazine
    hydrate boils at 117° C to 119° C. The forerun contains the excess
    water. It should be converted back to hydrazine sulfate by addition of
    sulfuric acid as done in step one. The yield is 10 grams of hydrazine
    hydrate.

    During the fractional distillation, there are some precautions
    which should be followed. Hydrazine hydrate attacks rubber and cork,
    so the use of these materials must be avoided in the distillation. It also
    attacks most kinds of stopcock grease. The distillation is most safely
    done under nitrogen. Nitrogen should be introduced into the distilling
    flask, and the system flushed of air for about 15 minutes. Then the
    rate of nitrogen flow is reduced, and distillation commenced. The
    product will also attack glass, albeit slowly. It should be stored in 304 or
    347 stainless steel. 316 stainless is not acceptable.

    Step Three:
    Anhydrous Hydrazine

    100 grams (100 ml) of hydrazine hydrate is mixed with 140 grams
    powdered sodium hydroxide. The apparatus is thoroughly flushed
    with nitrogen, then the rate of nitrogen addition to the distilling flask is slowed, and fractional distillation is commenced through an
    efficient fractionating column of about 15 theoretical plates.
    Anhydrous hydrazine distills at 112° C to 114° C. Anhydrous
    hydrazine is obtained at 99%+ purity.

    Another method for producing anhydrous hydrazine exists which
    gives a higher yield of product, but it uses anhydrous ammonia and
    more complicated glassware and procedures. See Journal of the
    American Chemical Society Volume 73, page 1619 (1951), and
    Volume 76, page 3914 (1954). Also see Hydrazine by C.C. Clark, The
    Chemistry of Hydrazine by L.F. Audrieth, and Industrial and
    Engineering Chemistry Volume 45, pages 2608 and 2612 (1953).
    Also see Inorganic Syntheses Volume 1, page 90 (1939).
    Anhydrous hydrazine can be stored in dark glass bottles under
    refrigeration for years.

    Other variations on the alkali hydroxide dehydration of hydrazine
    hydrate exist which give higher yields of less-pure hydrazine. See
    pages 48-54 in the Chemistry of Hydrazine mentioned above. It lists
    many references. Especially interesting is Journal of the American
    Chemical Society Volume 71, pages 1644-47 (1949).
    Preparation of Diethvlamine

    NH3 + CH3CH2I —s> xHI + CH3CH2NH2
    + (CH3CH2)2NH +
    (CH3CH2 ) 3N

    The reaction which produces diethylamine also yields as byproducts
    ethylamine and triethylamine. The relative amounts of each
    compound produced depends upon the molar ratio of the two starting
    materials. Use of only a little ethyl iodide favors the formation of
    mostly ethylamine. Use of a lot of the ethyl iodide favors the
    formation of triethylamine. Somewhere in the middle, a roughly even
    split occurs. This will be done here. See Journal of the American
    Chemical Society Volume 69, pages 836 to 838 (1947).

    A section of clean steel pipe 2l/2 to 3 inches in diameter is
    obtained, and fine threads are cut into each end so that a cap may be
    screwed onto each end. A really nice touch would be to have all the
    pieces plated with a half-thousandths-inch of electroless nickel, but
    the plater may think you are constructing a pipe bomb when he sees
    the pipe and caps.

    The bottom of the pipe is secured by screwing the cap on over
    threads coated with Teflon tape. Welding may also be used. The pipe is
    then nestled into a Styrofoam cooler, and is then filled about Vi full of
    rubbing alcohol, and then to this solvent dry ice is added, slowly at first
    to prevent it from boiling over, then more rapidly. The top of the pipe
    should be covered to prevent frost from forming inside the pipe as it
    cools down.

    Next, add 175 ml of ethyl iodide to the pipe, and let it cool down. It
    will not freeze, as its melting point is about 100° below O° C. Then liquid
    ammonia is added to the pipe. This is best done by inverting a cylinder
    of liquid ammonia, attaching plastic tubing to the valve, and cracking
    open the valve to feed the liquid into the pipe. About 525 ml of liquid
    ammonia is called for. In a 3-inch-diameter pipe, that plus the ethyl
    iodide will fill it half full. This is not an operation to be done in a
    residential neighborhood, as the fumes are tremendous. A rural setting
    with beaucoup ventilation is more proper.

    Now secure the top of the pipe by screwing on the cap tightly over
    Teflon tape. The pipe is now moved into a tub of ice water, and
    allowed to sit in this ice water for 45 minutes to an hour to warm up to 0°
    C.

    When the pipe has warmed to O° C, it should be shaken to mix the
    two reactants, and returned to the ice water. This shaking should be
    repeated a few times at 5-minute intervals. When 30 minutes have
    passed from the first shaking, the pipe should be returned to the dry
    ice bath and allowed to cool.

    When the pipe has cooled, the cap on the top of the pipe is
    loosened. Then the pipe is returned to the tub of ice water, and the
    ammonia is allowed to slowly evaporate away. This will take
    overnight, and raise great plumes of stink. After most of the ammonia has evaporated, the contents of the pipe should be emptied into a beaker. The foul substance is a mixture of ammonia, ethlyamine, diethylamine, triethylamine, and the hydriodides thereof. The best route to follow is to cool this mixture in ice, and slowly add with stirring 90 grams of sodium hydroxide dissolved in 100 ml of water. This neutralizes the HI in the mix, yielding the freebases of all.

    This mixture should be extracted several times with toluene.
    Toluene is chosen because it is available at the hardware store, and its
    boiling point is higher than any of the amines. The extracts should be
    filtered, and dried over sodium hydroxide pellets.

    The toluene extracts should then be transferred to a flask, and the
    mixture fractionally distilled through an efficient column. Ethylamine
    distills at 16° C, diethylamine distills at 55° C, and triethlyamine
    distills at 89° C. The diethylamine fraction should be collected over a
    20-degree range centered on 55° C, and this fraction then redistilled to
    get the pure product. The yield of diethylamine is about 40 ml.
    Absolute freedom from water in the product can be assured by letting
    the crude distillate sit over a few chips of KOH for a few hours prior to
    the final distillation.

    Preparation of Tartaric Acid

    My experience with the chemical scrutinizers while ordering a
    pound of Rochelle salts should serve as a lesson to those embarking
    upon LSD manufacture. Substances which are useful for this purpose
    will raise red flags if obtained through normal channels. It must then be
    the highest priority to avoid these normal channels, or to subvert their
    scrutiny by preparing yourself those substances with direct use in the
    synthesis.

    The most low-profile method for getting tartaric acid is to follow
    the procedure given below. It uses cream of tartar from the grocery
    store and gives good results. See Chemical Engineering Progress
    Volume 43, page 160 (1947). Also Organic Syntheses Collective
    Volume 1 for alternate procedures. I worked out this procedure by myself in my lab, and it gives good results. That such a simple procedure,
    using such easily obtained materials, so effectively subverts the feds'
    control over tartaric acid shows what a bunch of ninnies they really are.
    To make tartaric acid suitable for use in making the tartaric salt of
    LSD, weigh out 10 grams of cream of tartar, and put it into a 100 ml
    beaker. I used McCormick brand, and it was nicely white and fluffy.
    Other brands will do, so long as they too are white and fluffy.
    To the 10 grams of cream of tartar, add water until the 50 ml mark is
    reached in the beaker. This produces a milky white suspension. Stir for a
    while to try to dissolve as much as possible, then add 10 ml 37% labgrade
    hydrochloric acid. The mixture of calcium tartarate and potassium
    hydrogen tartarate that comprises cream of tartar reacts to form tartaric
    acid, along with KC1 and CaCl2- A clear solution results after about a
    minute of stirring.

    Now the water and excess hydrochloric acid are removed by vacuum
    evaporation. It is preferable to use a vacuum here, as heating at normal
    pressure may result in isomerization of the tartaric acid, and the
    replacement of some of the hydroxyl groupings in tartaric acid with
    chlorine. Also, hydrochloric acid was used here instead of sulfuric
    because the reaction is much faster, and the excess HC1 is removed
    during the evaporation. The solution should be evaporated down to a
    volume of about 10 ml. It will be yellowish in color, and have crystals of
    tartaric acid floating around in it, along with KC1 and CaCl2.
    Next, add 100 ml of 91% isopropyl alcohol, and dissolve the crystals
    of tartaric acid. KC1 and CaCh will not dissolve, and should be filtered
    out. 91% isopropyl alcohol is chosen because it is available at the
    drugstore, is not too good a solvent for tartaric acid for crystallization,
    and is less likely to form esters with tartaric acid than ethyl or methyl
    alcohol.

    The isopropyl alcohol is evaporated under a vacuum to 50 ml
    volume, and the first crop of white crystals of tartaric acid collected. This
    amounts to about 4 grams after drying. Further evaporation yields
    additional crops of crystals. Vacuum evaporation is used so that
    Practical LSD Manufacture

    heating does not contribute to the formation of the ester isopropyl
    tartrate.
     
  2. machinist

    machinist Banned Lifetime Supporter

    Messages:
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    lsd isn't synthesized in laboratories. a little fairy magically creates it and gives it to you when you're ready.
     
  3. L.ifes S.ubliminal D.ream

    L.ifes S.ubliminal D.ream Member

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    cool i just made lsd
     
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