JonnyDanger (Stranger)
07-16-03 21:29
No 447829
      GABA ---> NaGHB in layman's terms     

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 smile

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

Thanks to Chromic, fierceness, Rhodium, and all who have contributed to this write up in the post Post 394630 (Chromic: "Success making GBL!", Chemistry Discourse)
 
 
 
 
    fierceness
(Hive Addict)
07-16-03 22:31
No 447837
      nitrosamines should not be present in the last     

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
(Stranger)
07-16-03 23:27
No 447848
      The last step was a suggestion provided by...     

The last step was a suggestion provided by hCiLdOdUeDn so I will let him comment on that.
 
 
 
 
    JonnyDanger
(Stranger)
07-19-03 06:31
No 448381
      EDIT: step 10     

The DCM is boiled off at 40C
 
 
 
 
    JonnyDanger
(Stranger)
07-19-03 23:35
No 448483
      EDIT: step 5     

A hot water bath can be applied to speed up the process once the rxn has calmed.
 
 
 
 
    JonnyDanger
(Stranger)
07-20-03 14:56
No 448633
      A word of advice...     

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
(HyperLab Bee)
07-21-03 05:49
No 448753
      It is not working     

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.

With best regards,
Dennis Prochko aka Wolf
 
 
 
 
    JonnyDanger
(Stranger)
07-21-03 11:50
No 448784
      Its been tested     

Tried and true...
 
 
 
 
    methyl_ethyl
(Hive Bee)
07-21-03 19:07
No 448832
      It's been tested?     

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. frown  It sure would be great to supply the hive with a final write up complete with certificate of analysis.  laugh

     Unipolar Mania, It's good for life... laugh
 
 
 
 
    JonnyDanger
(Stranger)
07-21-03 22:53
No 448879
      That is correct     

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
(Hive Addict)
07-22-03 01:22
No 448912
      exactly     



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
(Hive Bee)
07-22-03 06:51
No 448970
      Is this it?     

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.

     Unipolar Mania, It's good for life... laugh
 
 
 
 
    JonnyDanger
(Newbee)
08-08-03 02:05
No 452365
      3-butyrolactone     

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...

One sec, now I have to shit again...
 
 
 
 
    StraightEdge
(Hive Addict)
08-08-03 02:31
No 452368
      what needs to be done to find out?     

This post Post 394630 (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
(Stranger)
08-15-03 12:01
No 453698
      In step 4, what is this Very Poisonous Gas?     

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.

Hi mom!
 
 
 
 
    StraightEdge
(Hive Addict)
08-15-03 19:56
No 453771
      ????????????     

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
(Newbee)
08-16-03 01:52
No 453814
      A few changes made. Most recent synth.     

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.

One sec, now I have to shit again...
 
 
 
 
    StraightEdge
(Hive Addict)
08-16-03 06:03
No 453845
      Very Poisonous Gas     

The gas that is produced in step four is nitric oxide (Post 394630 (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
(Hive Bee)
08-16-03 12:40
No 453899
      nitrous fumes     

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 blush) 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 pneumoniawink. I immediately went outside  to breath fresh air of course.

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

A Dream Within A Dream (http://www.poedecoder.com/Qrisse/works/dreamw.html)
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
08-19-03 06:37
No 454465
      Nasty gas     

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.
 
 
 
 
    JonnyDanger
(Newbee)
08-29-03 10:43
No 456325
      Yes, thank you Chromic.     

Yes, thank you Chromic. Thats why it says DISTILL off the DCM, not boil it off into the air... its quite nasty. BUT!!! I must say, SWIM has tried this process a few times now and has never gotten a product worth writing home about. Whenever SWIM has ingested what this synth makes, it feels like taking maybe 1 and 1/2 caps of normal potency GHB (1.5 grams powder) no matter how much SWIM ingests... which leads SWIM to believe that this process might in fact be producing beta hydroxybutyric acid, not GAMMA hydroxybutyric acid... I know that beta butyrolactone is a known carcinogen but do not know that much about beta hydroxybutyric acid but I dont think it can be very good for you... but I actually have no idea what im talking about and could very well be completely wrong, but it my guess (and it is only a guess) that the reason it always tastes wierd is b/c thats how beta hydroxybutyric acid is supposed to taste... and since finding a otc source of GBL, SWIM has no use for this synth so hasnt worked on it any further... but please, do not msg me asking for SWIMS source b/c I can not give it to you. Even though SWIM is one of the biggest GHB advocates you will ever meet, and would love to give the source out to everyone, he can not knowing that some of you ppl might be undercover piggy pigs. Just do some research for yourself!!! Eventually you will come across it, and if you do, msg me and I'll tell you if youve found the right stuff and what to do with it once you have. Live long and prosper.

One sec, now I have to shit again...
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
08-30-03 22:52
No 456514
      Definitely GBL     

This stuff is definitely GBL. It boiled at the right temperature and also put me into a coma fully reminiscent me of what lab-grade stuff used to do for me. You're absolutely right about the taste--there is something completely wrong with the odor. The GBL also tasted "sour" which was very odd.
 
 
 
 
    carcrash
(Hive Bee)
09-24-03 07:48
No 460673
      Adding a wash or 2?     

What about adding a baking soda wash then salt wash to the dcm mixture as step 9.5 before distillation?

I am guessing a trace of unreacted sulfuric acid or impurties in it is coming over.

Not a chemist I just follow directions on the box mix
 
 
 
 
    Rhodium
(Chief Bee)
09-24-03 17:21
No 460737
      sulfuric acid won't distill at that temp     

No, sulfuric acid doesn't come over at that temperature unless the distillation fails through exessive bumping and things splash over into the reciever from the distillation flask, in which case you need to start over anyway.
 
 
 
 
    chiliuno
(Hive Bee)
09-26-03 08:38
No 461153
      i have access to some analytical equipment,...     

i have access to some analytical equipment, and i've got a fellow cook for a ta in a spectroscopy lab i'm taking; i'll order reagents by the end of the weekend, synth sometime shortly after, and will have a detailed analysis by next fri. morning in all likelyhood.
i'm still new to the game; is there anything specific i need to ask, or do i just bring a sample to the ta?

i used TFSE...just answer TFQ!
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
09-27-03 07:53
No 461300
      GC/MS     

We need someone with access to GC/MS to run a sample of the product... stay in school chiliuno...
 
 
 
 
    shockwave
(Stranger)
11-12-03 21:51
No 470530
      A Few Changes Needed     

A. Gloves should be worn throughout the entire process. This is obvious but some people might not be so intelligent.

B. Sulfuric acid needs to be handled with extreme care even when not being used in conjunction with other materials. Again, very self evident.

C. DCM is very hazardous also. Even on "Safe Surfaces" it will still leave marks.

D. For .5 mol synths, 250 ml of dcm (5 shakes at 50 ml) will yield 31 ml of crude and 500 ml (5 shakes at 100 ml) of dcm will yield 34 ml. 10% increase

E. Propane distillation of dcm will decide which amount of dcm to use. 250 ml will require 30 mins and 500 ml will require 45 mins.

F. DCM returns will be very low or distillation will take a long amount of time unless a proper distill setup is arranged. One may use a coil condenser. With a regular condenser and a ice bath set up, 30 mins for 250 ml of dcm and 45 mins for 500 ml of dcm is required. 15-20% dcm loss is around the average attained.

G. Ph Balencing with NAOH is no joke. The steam is dangerous.

When reading this thread, one may think it is very simplistic. It's not. I weap for the amount of damage done to a person's home. Sulfuric acid eats through everything. Old clothes will become trash. Nitrite and NAOH will discolor skin easily. DCM will do worse. And people who use propane will sometimes forget the amount of Carbon Monoxide produced.




Bottom Line: Cuts Heal, Chicks Dig Scars, and Glory Lasts Forever

Never Speed Up The Process. Even if bubbles are not visible, they are still there. If a clear reagent grade sulfuric is used, it will be evident. You may receive a high yield but it will be crap. Do it right