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Synthesis of ghb (free acid) from gbl

- Tue, 18 Jul 2017 22:06:27 EST 1reNg8pO No.78749
File: 1500429987701.jpg -(42696B / 41.70KB, 500x345) Thumbnail displayed, click image for full size. Synthesis of ghb (free acid) from gbl
I recently came across some lab grade gbl (gammy-butyrolactone) which is the precursor to GHB. I've got a few questions because I've never find GH and I'm having a hard time finding some info from chemists who know what they're doing.

Firstly, I wanted to make GH in its free acid firm, rather than the common sodium butyrate salt. What I want to know are whether its fine to take it in free acid form. I think the pka is about 4, so it shouldn't be too sour if diluted in water, but taking it in free acid produces the same effects right? I assume that taking the sodium salt would Judy result in it finding in the acidity of the stomach anyways, I just would prefer to not have to eat a bunch of salt on the side.
Also, did I do something wrong in my procedure?

I started with about 10g gbl weighed analytically, and calculated the moles for sodium hydroxide which was between 6-7g, but I put in some excess to try to push the reaction forward.
I then added a bit of water, roughly 20mL in a round bottom flask, added the hydroxide and then the gbl. After a few minutes, I capped the flask and put it in an oil baths at 70 celcius.
After 2-3 hours, I added a bit of hydroxide to make sure the reaction was basic and he GH would be in its salt form, then I washed the solution with ether 3x to get rid of any remaining unreacted gbl. I took the aqueous layer and added HCl from a 1M solution until the pH was about 2-3, low enough for the gh to be in its acid form. I think the problem is here, because I couldn't find concentrated acid so I ended up adding a lot of water on the side..
Then my last step was to extract the ghb from the autos later with ether. I did this about 3x, combined the etherI'm layers, and evaporated off the ether. I was left with 2g when theoretical yield should have been about 12g.

Do you think that because I ended up using so much water, my remaining gh is in the aqueous solution? I know theree acid is readily soluble in both water and ether, so I'm wondering if this is my problem.

Also, how can I test the solution to show I have ghb with no gbl? I don't want to use the NMR spectrometer just in case somebody ends up seeing the spectrum and asking questions
Matilda Chommlekog - Tue, 18 Jul 2017 22:10:40 EST 1reNg8pO No.78750 Reply
Sorry about all the spelling/grammar errors, I wrote this on the bus on my phone and it autocorrected way too much.
I meant to write the sodium salt just converts into the free acid in the stomach, so taking the free acid should produce the same effects as taking the salt right?
Lydia Clannerfeck - Thu, 20 Jul 2017 17:47:14 EST UoTssc8h No.78751 Reply
ayy so GBL is a prodrug to GHB. You could just eat the GBL.

Keep extracting the aqueous layer. There's probably more in there. Also try adding some salt (NaCl) to the water to lower the solubility of the GHB in it.

You can tell if there's any GHL in it by taste. GHL supposedly tastes awful whereas GHB is tasteless.
press !XIxc6BpKnU - Sat, 22 Jul 2017 18:28:22 EST PJ0/E4z+ No.78753 Reply
ghb has a distinct taste too, it just isnt as fucking horrible as gbl
somewhere between gasoline, coconut and soap
OP have you considered to simply mix the gbl with a sodium carbonate solution to get a ready to use sodium ghb solution.
obviously youd have take in more volume but it always worked for, although getting too much sodium isnt too healthy and the sodium salt gave me just as much diarhea as gbl.
since the sodium salt is hygroscopic anyways youd have to hustle to keep it dry

Cyril Sunnertot - Mon, 24 Jul 2017 16:41:05 EST CwYciqLe No.78754 Reply
Thanks for the replies everyone. I found a paper and read that ghb is rarely found in its free acid form as it readily converts back to GBL. This back conversion happens even more easily in acidic conditions, which I used to try to protonate the free acid. I will extract as much of what is most likely gbl now from my aqueous solution using salt to push it to the organic layer, evaporate any ether and water left over and mix the gbl back with a small excess of sodium hydroxide. I'll calculate it so that once all the gbl had reacted with the sodium hydroxide in a 1:1 stoichiometric fashion, that the pH will be about 8.5 at the end in a small precculated volume so the ghb doesn't convert back to gbl

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