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GHB Synthesis


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#1 aushy

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Posted October 01 2009 - 05:05 AM

I've found this synthesis for GHB which uses all readily available chemicals. What do you guys think of it? Also, I've heard that GBL can be made from tetrahydrofuran, except i can't seem to find a synthesis.. anybody have a source? Or does anybody know of any other methods to make GBL?

This is from http://www.drugs-for...y/gaba2gbl.html


Sandmeyer Reaction of GABA to GBL/GHB

by Chromic
Quick introduction

As other writeups that I have published, this method is 100% OTC. It is awesome for a chemist who wishes to prepare GHB in small quantities and high yields and to do so without directly obtaining any regulated chemicals such as gamma-butyrolactone (GBL) or 1,4-butanediol (BDO). It also avoids the typically low yields seen from the oxidation of tetrahydrofuran (THF). It uses an easy to obtain amino acid, gamma-aminobutyric acid (GABA), and sodium nitrite (NaNO2). It scales very nicely and runs without too much hassle. Not one suspect chemical is used.

The Sandmeyer reaction uses nitrous acid to turn amines into diazonium salts. This reaction, as it applies to turning GABA into GHB, is shown in the first reaction below. Aliphatic diazonium salts rapidly undergo hydrolysis in the presence of water giving off nitrogen gas and leaving a hydroxyl group behind. This is shown in the second step. As a result of these reactions, GABA can be turned into GHB in an easy to perform one-pot reaction.
Running the reaction

Set up a 2L flask, sitting in ice-water on top of a magnetic stirrer. Now:

1. Add 3mol GABA (309.4g)
2. Add 3mol NaNO2 (207.0g)
3. Add 700ml water (total volume becomes about 1100ml)
4. Drop in a 1" stir bar and start stirring
5. Charge a 500ml pressure equalized addition funnel with 3.3mol HCl(aq) (385.0g 31.25%, 334.8ml 31.25%)
6. Fit the addition funnel with a gas outlet adapter and vent to theoutside

Begin slowly dripping the hydrochloric acid into the mixture. Drip it in at a constant rate of about 1 drop every 2-5 seconds. Speed it up as time progresses and replace the ice as necessary, but do not allow the evolution of the brown poisonous gas to become vigorous. After about one hour after the last drop of acid has been added, there is no need to replace the ice. Once the reaction is done, proceed to extract. (usually 24-36 hours later)
Extracting the goods

There are many options for this. This is still a work in progress, but after about 20 runs, I came to use this work up. You can use ethyl acetate (EtOAc), chloroform or methylene chloride (dichloromethane aka DCM) to perform the solvent extractions. I have normally used DCM as it's nice since the organic layer drops to the bottom of the separatory funnel.

1. Setup for a simple distillation.
1. Distill, throwing out the first 5-10mls, or so, of distillate as it will contain a fair amount of nitric oxides. Distill off as much water as possible, basically until the sodium chloride starts to saturate the aqueous layer and precipitate out.
2. The remainder of the distillate (approximately 700ml) will contain approximately 1g GBL/10ml.
3. Treat the remainder of the distillate with NaHCO3 at reflux for 30 mins
4. Boil with about a 5% volume of activated charcoal (ie 35ml activated charcoal) (compared to the volume of the solution) for 5-10mins.
5. Allow it to cool and filter, wash the charcoal with distilled water. Save the NaGHB.
2. With the remainder of the aqueous, extract 5 times with 625ml portions of DCM.
3. Distill off the DCM (reuse that DCM!).
4. Distill the GBL (under vacuum if available).
5. React with NaHCO3 and distilled water and treat with activated charcoal as before.

Typically 375g of NaGHB is made from the solvent extracted GBL and 100g NaGHB from the aqueous distillate. Although conversion is nearly quantitative (as measured by GC/MS), the overall recovered yield is usually about 70%.

For those who don't know how to make NaGHB from GBL using NaHCO3 please read the section on preparation of Sodium GHB using Sodium Bicarbonate (Baking Soda, NaHCO3) found in the GHB faq. Never use unknown grades of NaOH--they may contain toxic heavy metal contaminants.

OTC chemicals rock. The war is over.

Notes on procedure

* 1M NaNO2/GABA, as the French ref states is far, far too much water. You don't need it. I don't use that much.

* It's possible to reduce the water further, down to the minimum necessary to dissolve the NaCl formed, thus avoiding the distillation of the aqueous layer. The trouble with this is that it's not fully practical. All of the GABA/NaNO2 will not dissolve, and you'll see more of an evolution of nitric oxides. The amount of water used is just barely enough to dissolve all of the NaNO2 and GABA to begin with.

* If you want to skip the simple distillation (steps 1a-e) and go straight to step 2 (the extraction with the organic solvent) make sure to increase your organic solvent amounts by about 20%. Your yields will go down slightly.

* It's possible to used sulfuric acid, however Na2SO4 is not as soluble as NaCl is, mole for mole. You'll need to use more water.

* It's possible to use just a little bit less HCl, but hey, a slight excess is always a good idea.

* It's possible to dump in a fair amount more HCl to try and push the GBL into the organic layer. It doesn't really work that well though. Yields don't go up.

* It's possible to use chloroform or ethyl acetate instead of dcm. Diethyl ether will work as well. Do not try to use anything more nonpolar such as toluene, hexanes or the like. They won't extract much GBL.

* Figuring out where the other 30%+ of the yield is going has been frustrating. Perhaps it is staying in the aqueous as free GHB. But do not consume the post-reaction aqueous layer!

* The GBL produced from distillation has an putrid sour smell. This is likely trace quantities of butyric acid (the molecule responsible for the smell of rancid butter). It is not toxic in trace quantities and the off-smell and off-taste is cleared by treatment with activated charcoal.

* The dose/response curve for NaGHB is exponential. 2g may be a nice buzz, 2.5g an amazing high, and at 3g a novice user could be violently ill, passed out and completely unresponsive. These doses are guidelines. Every person's response will vary. Chronic use of GHB will result in tolerance and physical addiction. Never mix with any other CNS depressants (especially alcohol).

#2 36fuckin5

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Posted October 01 2009 - 08:12 AM

I didn't read it, but I already saw a problem. It's telling you to add H2O to NaOH. This is WRONG and can get you KILLED.
I stared God in the face and asked his name. He tickled from the tips of my toes to the tip of my head. I knew then that it didn't matter.

#3 shermin

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Posted October 01 2009 - 03:25 PM

seriously...basic rule of thumb "add dangerous shit to water...NOT water to dangerous shit"
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#4 aushy

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Posted October 01 2009 - 05:03 PM

I didn't read it, but I already saw a problem. It's telling you to add H2O to NaOH. This is WRONG and can get you KILLED.


Thanks for the tip, but I did already know this. Although I can't seem to find where it says this in procedure.

#5 36fuckin5

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Posted October 01 2009 - 10:45 PM

Set up a 2L flask, sitting in ice-water on top of a magnetic stirrer. Now:

1. Add 3mol GABA (309.4g)
2. Add 3mol NaNO2 (207.0g)
3. Add 700ml water (total volume becomes about 1100ml)


If they aren't careful enough to NOT tell you to add water to powdered lye, I wouldn't trust that they're careful enough to get this right.
I stared God in the face and asked his name. He tickled from the tips of my toes to the tip of my head. I knew then that it didn't matter.

#6 aushy

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Posted October 02 2009 - 02:34 AM

If they aren't careful enough to NOT tell you to add water to powdered lye, I wouldn't trust that they're careful enough to get this right.


Hmm that is a good point.
Is there any method which would test GHB purity? I think it would be doubtful short of $1000s woth of equipment :S

Does anybody know of any other methods to make GHB without using GBL?
Or does anybody know any methods to make GBL?

#7 36fuckin5

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Posted October 02 2009 - 09:08 AM

Hmm that is a good point.
Is there any method which would test GHB purity? I think it would be doubtful short of $1000s woth of equipment :S


You'd think so, but a TLC plate ran against a known sample would do you just fine for almost nothing.

Does anybody know of any other methods to make GHB without using GBL?
Or does anybody know any methods to make GBL?


No, on both counts, and you're asking in the wrong place. I'm sure Google has a guide.
I stared God in the face and asked his name. He tickled from the tips of my toes to the tip of my head. I knew then that it didn't matter.

#8 LSDMIKE

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Posted October 02 2009 - 03:47 PM

I didn't read it, but I already saw a problem. It's telling you to add H2O to NaOH. This is WRONG and can get you KILLED.


No you must be kidding yer!

#9 LSDMIKE

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Posted October 04 2009 - 04:09 PM

man i was mixin this stuff at the age of ten.

in australia pre-drying treatments that hasten drying are used. Sultanas are dipped in or sprayed with an alkaline oil-in-water emulsion known to growers as 'cold dip'. The commercially produced 'grape dipping oil' used in the emulsion is a mixture of ethyl esters of fatty acids and free oleic acid.
This is emulsified in a solution of potassium hydroxide's in water. The standard cold dip solution is made up of 2.4 kg of Potassium hydroxide and 1.5 litres of dipping oil in l00 litres of water.

The only way it can kill you is if you eat 4 gallons of it in six minutes :D

#10 arcdemon

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Posted January 09 2010 - 11:57 AM

Hmm that is a good point.
Is there any method which would test GHB purity? I think it would be doubtful short of $1000s woth of equipment :S

Does anybody know of any other methods to make GHB without using GBL?
Or does anybody know any methods to make GBL?



there are several ways of manufacturing ghb without directly using gamma butyrolactone. one method that completely avoids the use of gbl is the diazonium salt production of GABA. This is called the Sandmeyer reaction. It involves reacting gaba with nitrous acid formed in situ from sodium nitrite and hydrochloric acid. Compared to other methods it involves a definate degree of danger due to the formation of nitric oxide gases but in my experience at small scale it is not all that perilous. Essentially gaba is dissolved in water with sodium nitrite and the hcl is slowly dripped in, once the addition is complete it is let sit for about a day to allow the water to hydrolyse the nitrogen leaving behind the hydroxl which is characteristic of GHButyric acid (this is done in acidic conditions so you don't get the butyrate you get the acid) You then steam distill off the product which is gbl since the butyric acid does not like to exist on its own so it forms the lactone. It is about 10% gbl in water. You want to run it over activated carbon and or silica to remove the smell of butyric acid which smells like rotten butter.

Of course everyone knows about butandiol so i would sound like a wanna be trying to sound like i know something to even mention it.

Tetrahydrofuran can be oxidized in several ways to gbl but I have never really looked to far into any of them. Nitric acid, calcium hypochlorite, cyanuratic acid based pool shock and some other strong oxidizers can do the job but don't attempt any of them.

In my opinion ghb isn't even worth the effort of a synthesis or at least going to too much trouble to synthesize it, you're better off just getting drunk or sniffing gas or something, you have a less chance of poisoning yourself that way than using the sandmeyer reaction or nitric acid to make ghb. If you must there is a canadian chemical company more than happy to help anyone out with whatever they need but i don't know if i can give it out on the forum.

#11 arcdemon

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Posted January 09 2010 - 11:58 AM

my apologies to the gentleman above who posted chromics sandmeyer, i didn't see that.


there are several ways of manufacturing ghb without directly using gamma butyrolactone. one method that completely avoids the use of gbl is the diazonium salt production of GABA. This is called the Sandmeyer reaction. It involves reacting gaba with nitrous acid formed in situ from sodium nitrite and hydrochloric acid. Compared to other methods it involves a definate degree of danger due to the formation of nitric oxide gases but in my experience at small scale it is not all that perilous. Essentially gaba is dissolved in water with sodium nitrite and the hcl is slowly dripped in, once the addition is complete it is let sit for about a day to allow the water to hydrolyse the nitrogen leaving behind the hydroxl which is characteristic of GHButyric acid (this is done in acidic conditions so you don't get the butyrate you get the acid) You then steam distill off the product which is gbl since the butyric acid does not like to exist on its own so it forms the lactone. It is about 10% gbl in water. You want to run it over activated carbon and or silica to remove the smell of butyric acid which smells like rotten butter.

Of course everyone knows about butandiol so i would sound like a wanna be trying to sound like i know something to even mention it.

Tetrahydrofuran can be oxidized in several ways to gbl but I have never really looked to far into any of them. Nitric acid, calcium hypochlorite, cyanuratic acid based pool shock and some other strong oxidizers can do the job but don't attempt any of them.

In my opinion ghb isn't even worth the effort of a synthesis or at least going to too much trouble to synthesize it, you're better off just getting drunk or sniffing gas or something, you have a less chance of poisoning yourself that way than using the sandmeyer reaction or nitric acid to make ghb. If you must there is a canadian chemical company more than happy to help anyone out with whatever they need but i don't know if i can give it out on the forum.



#12 LSDMIKE

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Posted January 16 2010 - 07:30 AM

Tetrahydrofuran (THF) where do you think you can buy this from?

#13 yesnomaybe

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Posted May 09 2011 - 04:22 PM

what company arcdemon pls pm me

#14 LSDMIKE

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Posted June 13 2011 - 06:07 AM

nvm

#15 PurpByThePound

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Posted December 05 2012 - 11:45 PM

Why the fuck?

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#16 Tikalite

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Posted February 27 2013 - 06:26 PM

If they aren't careful enough to NOT tell you to add water to powdered lye, I wouldn't trust that they're careful enough to get this right.

That is Sodium Nitrate a safe food additive not Sodium Hydroxide. It doesn't matter which you dump in first in this case.

#17 Tikalite

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Posted February 27 2013 - 06:30 PM

Tetrahydrofuran (THF) where do you think you can buy this from?


It can be purchased or distilled from PVC pipe cleaner. When purchasing it just say you need it to fuze rubber sheeting together if asked. It's always good to know what chemicals are normally used for before attempting to buy them. If you are just a kid it may be a problem, otherwise just act like you are in a rush to get a job done and don't have time to bullshit with the salesman or rep.