GABA ---> NaGHB in layman's terms

[JonnyDanger]

I'll try to explain the method in layman's terms as I understand it... The highest lvl of chemistry education I have is highschool but I've read all the posts and have done much research as well... so here goes:
(Any suggestions, modifications, or corrections to the following method would be much appreciated.)

Ingredients needed (which can all be purchased online on various websites):
154.7g pure GABA, 103.5g Sodium Nitrite, 225.2g Sulfuric acid, 750ml DCM, 90.1g baking soda (or Sodium Hydroxide, not sure on exact amount though) and Distilled water.

Equipment needed (All of which can also be purchased online):
high temp thermometer (at least 210c max temp), 1 1L capacity, flat bottom Erlenmeyer flask, 1 distilling set up, 1, 1L capacity seperatory funnel (for the separation process and the acid dropping process), 1 Bunsen burner or similar heating apparatus (a propane torch maybe?) one large bowl (at least 3L capacity), PH testing strips, and safety equipment (i.e. safety goggles, gloves, apron).

PROCESS:

1: In the 1L Erlenmeyer flask, mix the GABA, Sodium Nitrite, and 750ml water.

2: Set that mixture (inside of the Erlenmeyer flask) in the large bowl with water and ice and allow to cool.

3: In the separatory funnel, add about 120 ml ICE COLD water. Then SLOWLY add 75.1g sulfuric acid.

4: Rig the separatory funnel so that its above the Erlenmeyer flask and may drip into it. Allow the sulfuric acid mixture to slowly drop into the GABA/Sodium Nitrite mixture (NO MORE THAN ONE DRIP/SECOND and no more than 20ml/hour). NOTE: This process should be done outside or with very adequate ventilation as a VERY poisonous gas is produced by the reaction.

5. Let sit for 24 hours or until no more bubbling is seen.

6. Add another 150.1g of sulfuric acid to the mixture. (Not sure one the addition time or if water should be mixed with the sulfuric acid first... some help here?) Let sit for 6 hrs.

7. Clean the separatory funnel.

8. In the separatory funnel, mix 150ml DCM and the GABA/sulfur/sodium mixture and shake well.  Allow to sit until separation can be seen (2 layers of liquid). Remove the DCM portion and SAVE. It will be the bottom portion. With the remaining portion, again add 150ml of DCM and shake. Again, remove the DCM/GBL portion. Repeat 3 more times. (if any part of this step is wrong or could be explained more clearly, let me know and I will modify it.)

9. Combine the multiple DCM/GBL separations.

10. Boil off the DCM (at approx 100C?) till only the GBL remains (which should be yellow/brown liquid).

11. (optional, for added purity and enhanced taste) Simmer the GBL at 100C with approx. 3-5g of activated charcoal while stirring vigorously (magnetic stirbar recommended) for about 5 minutes.  Then filter through a 5mm thick layer of celite.

12. Distill the GBL in your distilling apparatus at 198-202C. (If someone wants to make a full write up of the distilling process I will add it).

13. Mix 90.1g baking soda and 370ml distilled water.

14. Simmer GBL and baking soda mixture at 100C for 30 min to balance the PH by forming NaGHB. (I prefer to use NaOH for this step)

15. Redilute with water to desired potency.

-----------------------------------------------------------

Once again, pls let me know of any suggestions or mistakes/misleading statements as I have just woken up so I'm sure there will be  

----------------------------------------------------------

Thanks to Chromic, fierceness, Rhodium, and all who have contributed to this write up in the post

Post 394630 (missing)

(Chromic: "Success making GBL!", Chemistry Discourse)

[fierceness]

nitrosamines should not be present in the last step if you added conc H2SO4 after the 24hr rxn..  where do you get that activated charcoal removes nitrosamines?  I have not read that anywhere.. only that strong acids destroys them

[JonnyDanger]

The last step was a suggestion provided by hCiLdOdUeDn so I will let him comment on that.

[JonnyDanger]

The DCM is boiled off at 40C

[JonnyDanger]

A hot water bath can be applied to speed up the process once the rxn has calmed.

[JonnyDanger]

After watching SWIM perform this rxn (and this is probably a pretty obvious statement), I must say, TAKE YOUR TIME... Good things come to those who wait and even better to those who wait longer... Dont try to rush anything and do a pratice run of every step in the process b4 attempting the real thing...

Oh and EDIT step 4: Let the sulfuric acid mixture drop in at 1 drop/5 seconds, not 1... once a second proved to be a too fast.

[dennis_pro]

You can't make GHB from GABA/nitrite, due rearrangement, it produces CH3-CH(OH)-CH2-COOH. I have tried to make GHB from GABA/nitrite year ago, w/out success.

[JonnyDanger]

Tried and true...

[methyl_ethyl]

Its been tested. Tried and true...

    As far as I know it has not been "tested".  It seems many bees have worked the synth and bioassayed, and even experienced satisfactory results, but, no one really knows for sure if what is produced is actually "pure" substance.  IMHO analytical analysis, will be the only way to know if what we have is what we "think" we have.  I would hate to think that everyone is poisining themselves through some unknown impurity due to this synth.

     If I had time I would love to figure out how to use all of the analytical equipment I have access to.  But I fear the columns and libraries are all geared towards biologics, I am clueless in this area.     It sure would be great to supply the hive with a final write up complete with certificate of analysis.   

[JonnyDanger]

What you say is true Methyl, but I was just refering to the fact that it does produce GHB, not the final results purity...

[fierceness]

As far as I know it has not been "tested".  It seems many bees have worked the synth and bioassayed, and even experienced satisfactory results, but, no one really knows for sure if what is produced is actually "pure" substance.  IMHO analytical analysis, will be the only way to know if what we have is what we "think" we have.  I would hate to think that everyone is poisining themselves through some unknown impurity due to this synth.

Exactly the reason we didn't release a writeup.. maybe that rearrangement product is the foul tasting impurity in the GBL.. does anyone know the chemical data on that in comparison to GBL ?  BP, etc?

[methyl_ethyl]

Is this what we are looking at? 

3-Hydroxybutyric acid
CAS Number: 625-71-8
Formula: CH3CH(OH)CH2CO2H
Formula Weight: 104.10
Form: Liquid
Boiling Point: 130°/12mm
Merck Number: 13,4841
Refractive Index: 1.4445
Sensitivity: Hygroscopic
Flash Point: >112°(234°
Notes: Store cold
Solubility: Soluble in water, alcohol, ether




     If I am way off please let me know, this is not my area of study at all!! I just want to figure this mystery out, so people are not polluting themselves with known carcinogens.  Just trying to help....  There was also another CAS# 300-85-6  DL-B-HYDROXYBUTYRIC ACID FREE ACID however sigma claimed "Unstable! Forms bimolecular esterification products up to 35%.
See the sodium salt for a stable alternative."
     I hope I am on the right track, if not I am sorry, just trying to help out.

[JonnyDanger]

Were you able to find the boiling point for 3-butyrolactone? Its its significantly different from 4-butyrolactone we would know if thats what was being synthesized. In every test SWIM did the assumed GBL did distill at 204C...

[StraightEdge]

This post

Post 394630 (missing)

(Chromic: "Success making GBL!", Chemistry Discourse) seems to indicate ( "The bioassay is, without a doubt, ABSOLUTELY POSITIVE! The quality is the same as A.C.S. butyrolactone." ) that there is at least some GBL in the final product.

You say you have access to analytical equipment, correct? You would be doing a great service to all of us if you could figure out how to use it and test a sample of your final product. Even better would testing of two samples, one each from before and after boiling with charcoal. That way we would know if that step is removing that contaminant or not. I asked in another thread whether charcoal removes the bad taste, but so far nobody has replied.

I'm not asking you to put your balls on the line to do this. If you will get in trouble for testing an unknown substance, then please don't do it. But if things are pretty lax at your university/workplace, what are you waiting for?

[merbst]

In step 4, what is this Very Poisonous Gas?  Is it corrosive in addition to poisonous?  Would it damage an exhaust "box fan" running at high speed blowing it out the window?  Is it harmful to the environment?  Would it kill the plants outside one's window?  Could it be captured in activated charcoal?  Or some type of zeolite molecular sieve?  Could it be captured in a punching bag balloon?

Additionally in step 10 when one is boiling off the DCM, this is a carcinogenic substance, would it be feasable to distill this into another flask without risk of explosion or leak?

I personally would not consider a synth which lives up to the sterotype of dangerous home labs which pollute our environment and at risk of blowing up the neighborhood a complete synth.

[StraightEdge]

Do you ask too many questions? Do you not know how to use the search engine? Are you a pompous asshole who is acting like it is our job to only provide you with synths that are 100% risk free? Do you really think a little poisonous gas is going to blow up your neighborhood?

Is this synth listed on Rhodium's site? Was it posted by someone who seems to have a lot of chemistry experience? Has anyone with a lot of chemistry experience given it their seal of approval?

[JonnyDanger]

Ingredients needed (which can all be purchased online on various websites):
154.7g pure GABA, 103.5g Sodium Nitrite, 225.2g Sulfuric acid, 750ml DCM, 90.1g baking soda (or Sodium Hydroxide, not sure on exact amount though) and Distilled water.

Equipment needed (All of which can also be purchased online):
high temp thermometer (at least 210c max temp), 1 1L capacity, flat bottom Erlenmeyer flask, 1 distilling set up, 1, 1L capacity seperatory funnel (for the separation process and the acid dropping process), 1 Bunsen burner or similar heating apparatus (a propane torch with 3/4 intake holes covered works perfectly) one large bowl (at least 3L capacity), PH testing strips, 5G activated charcoal (found at your local vitamin store), a few grams of celite (found at a pool supply store sold as a filter aid), 1 bruchner funnel, some fine filter papers, and safety equipment (i.e. safety goggles, gloves, apron).

PROCESS:

1: In the 1L Erlenmeyer flask, mix the GABA, Sodium Nitrite, and 750ml water.

2: Set that mixture (inside of the Erlenmeyer flask) in the large bowl with water and ice and allow to cool.

3: In the separatory funnel, add about 120 ml ICE COLD water. Then SLOWLY add 75.1g sulfuric acid.

4: Rig the separatory funnel so that its above the Erlenmeyer flask and may drip into it. Allow the sulfuric acid mixture to slowly drop into the GABA/Sodium Nitrite mixture (NO MORE THAN ONE DRIP EVERY 5 SECONDS and no more than 20ml/hour). NOTE: This process should be done outside or with very adequate ventilation as a VERY poisonous gas is produced by the reaction.

5. Let sit for 24 hours or until no more bubbling is seen.

6. Add another 150.1g of sulfuric acid to the mixture and let sit for 6 hrs.

7. Clean the separatory funnel.

8. In the separatory funnel, mix 150ml DCM and the GABA/sulfur/sodium mixture and shake well.  Allow to sit until separation can be seen (2 layers of liquid). Remove the DCM portion and SAVE. It will be the bottom portion. With the remaining portion, again add 150ml of DCM and shake. Again, remove the DCM/GBL portion. Repeat 3 more times.

9. Combine the multiple DCM/GBL separations.

10. Distill off the DCM at approx 40C - 80C till only the GBL remains (which should be yellow/brown oily liquid).

11. Slowly distill the GBL in your distilling apparatus at 198-202C. (If someone wants to make a full write up of the distilling process I will add it).

12. Mix 90.1g baking soda and 370ml distilled water.

13. Simmer GBL and baking soda mixture at 100C for 30 min to balance the PH by forming NaGHB. (I prefer to use NaOH for this step)

14. Redilute then simmer the NaGHB with 5g of activated charcoal for a few minutes while stirring vigorously. Allow to cool then filter through 5mm thick layer of celite. Repeat up to 3 times for added purity.

15. Dilute with water to desired potency.

[StraightEdge]

The gas that is produced in step four is nitric oxide (

Post 394630 (missing)

(Chromic: "Success making GBL!", Chemistry Discourse)). But to give it the proper deference, it should only be referred to as "Very Poisonous Gas". It may get angry if you call it something like "Slightly Poisonous Gas" or don't capitalize its name.

The MSDS for nitric oxide can be found at

http://www.mwsc.com/MSDS/86.PDF

According to that document, Very Poisonous Gas is corrosive as well as poisonous. To deal with it, you can either blow it out the window (your plants should survive, unless you live in a cave), or bubble it through aqueous NaOH to produce aqueous sodium nitrite (

Post 264620

(PrimoPyro: "Re: Nitric Oxide", Chemistry Discourse)).

But it's not one of those things where the danger is exaggerated, and you can breath a little bit and still be okay. It is very deadly.

[Vitus_Verdegast]

But it's not one of those things where the danger is exaggerated, and you can breath a little bit and still be okay. It is very deadly.

I'm all with you in taking the necessary precautions. Contact with this gas should be avoided by all means.

But your last sentence is not entirely true, it's not like HCN or the likes. I have had a couple of accidents (HNO₃ incompatibles   ) in the past where a small amount of nitrous fumes were released in the air. Of course I immediately moved the container outside and ventilated the room very well, but nevertheless I inhaled a bit of it. Luckily no chemical pneumonia . I immediately went outside  to breath fresh air of course.

When working with nitrous gasses be careful! Take appropriate precautions!

[Chromic]

Well, I breathed in a fair bit of NOx in this synthesis. Breathing it in never killed me nor caused any lasting damage. It irritated my lungs and had a large cloud of this been formed (by carelessly adding the acid, for example) I'm sure I would have been coughing for days. It reminds me of a nastier verion of SOx.

Merbst, if you're freely boiling DCM off into the air, you're an idiot. Recycle all your solvents! You are expected to have a good understanding of chemistry and practical lab experience to follow a preliminary writeup like this.