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GHB solvents

L

Limpet Chicken

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Joined
Sep 12, 2004
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What solvents will GHB (sodium salt) dissolve in? SWIM wants instead of neutralising excess NaOH from the ring-opening of the GBL used with HCl, to take up the GHB in a solvent, and filter off any remaining NaOH.

Normally SWIM would form a freebase and extract with nonpolar solvents, but of course with GHB, that isn't possible, so, with it being a salt, I assume a polar solvent like MeOH or a ketone would work well?
 
^ Yes it is; only in this case you have to make the aqueous phase acidic to 'encourage' the GHB to move into the organic phase. All the solvents for GHB sodium salt are also going to dissolve NaOH (ethanol, other alcohols, water etc).

Acid base separation works whether the salt is an amine with an acid or a carboxylate with a metal ion, it's just that you have to use the opposite process when dealing with an organic acid as opposed to an amine freebase.

For bases (eg amines)
aqueous phase alkaline - amine moves into organic phase
aqueous phase acidic - amine moves into aqueous phase

For acids (eg GHB, barbiturates)
aqueous phase alkaline - acid moves into aqueous phase
aqueous phase acidic - acid moves into organic phase
 
Thanks, that is exactly what I wanted to know, I will acidify slightly with HCl, neutralising some of the NaOH whilst I am at it, then take up in DCM and distill off the solvent for reuse.
 
Maybe I'm missing something, but this seems a little unnecessary and potentially wasteful.

It is not hard to get the pH near neutral without adding HCl and if the pH is near neutral, the [OH] will be close to zero.
 
I haven't enough HCl left, to do the entire lot, so I figured, I will just distill some paint remover (DCM/MeOH) and use the combined distillate, it saves any messign around, the NaOH will stay where its put, but GHB will go into the organic layer, byzantine way to go about it, but should do the trick.

My point is, I don't want salt in there, it screws up taste, and dose calculation, a purer product is well worth a little loss, and the amount in question, is sufficient to make small losses inconsequential;)
 
Hold on, what pH are you going to go down to before you do the extraction? Unless you get down to at least 5 or less you're not going to extract much of anything, and chances are you're probably going to have to use a large amount of methylene chloride and plenty of extractions to get a useful amount of ghb out.
 
Well, I will outline my problem.

Lets just say someone, who of course, isn't me, is sitting with a bag full of freshly made GHB, but at the moment, it is at a waxy consistency, looks like crack rocks, and still has residual NaOH in it.

SWIM wants to get pure GHB in the end, so, what about an alcohol extraction? NaOH won't dissolve to any great extent in anhydrous alcohols, so SWIM was thinking, just dissolve in MeOH and filter off the NaOH.
 
wouldnt acidifying the aquous layer turn the GHB into gamma-butyrolactone which then in turn would go into the organic layer?
i doubt that thats what the threadstarter wants.
maybe set the pH near neutral and then recrystallise to purify?
 
Wait you've got anhydrous alcohol? If you've got anhydrous ethanol then I'd say just dry your material really well, preferrably in a dessicator under vacuum, and then do a recrystallization from ethanol. Assuming the residual amount of NaOH you speak of is just a fraction of the total mass of material you have it should stay solvated in the ethanol whilst the NaGHB crystallizes out. You could try it with methanol as well but I can't guarantee it'll work. Though if it doesn't at least methanol isn't a bitch to remove.
 
NaOH won't dissolve to any great extent in anhydrous alcohols
Click to expand...

I'm afraid it will in lower (methanol, ethanol) alcohols. You could extract the free acid, then dissolve it in an excess of sodium carbonate (washing soda) soln, then evaporate to dryness and extract with alcohol as sodium carbonate (& sodium bicarbonate) are both pretty much insoluble in alcohols

This is assuming that Na-GHB is soluble in alcohols
 
I decided, I will take it to neutral PH, with HCl, and then extract it with MeOH, as NaCl is quite definately insoluable.

F&B, I have seen very little change in NaOH prills added to anhydrous EtOH or MeOH, actually, I often use a few prills of NaOH to decolorise the dye in denatured alcohol, for washing purposes, and the individual prills to not appear visually, to be dissolved at all by the alcohol, so I think, that it just might work, at most, only traces are present in the GHB, only enough to burn on contact with the tongue (bad test for caustic bases, I know), so I will make the solution neutral to phenolpthaline, then wash with MeOH.
 
Maybe try experimenting on a small amount like <10% of your total product. Organic chemistry is the type of thing where a bit of patience goes a long way.
 
Yes, sodium hydroxide is soluble in methanol and ethanol. Just look up any document that summarizes its physical properties, like, say.... this one.

-InfiniteBITCH
 
Limpet Chicken said:
Well, I will outline my problem.

Lets just say someone, who of course, isn't me, is sitting with a bag full of freshly made GHB, but at the moment, it is at a waxy consistency, looks like crack rocks, and still has residual NaOH in it.
Click to expand...

Pure GHB will quickly turn waxy and greasy upon exposure to the moisture in the air. If you are sure there's still NaOH in there, you could add some GBL if available and take it to neutral pH. It would certainly be a simpler solution.
 
I've made Na-GHB from NaOH / GBL but last time after reading this,

All of the recpies that use NaOH to make G have the same problem the reaction
only goes about half way leaving lots of unreacted lactone in the mixture.

If you've ever had pure ghb or powder(pharm-grade) ghb you do notice a
difference in effects and also have less side effects(headaches etc.), also
there will be no smell at all in your ghb and the taste will be better if it
doesn't contain lactone. There are a whole slew of reasons for wanting g
without lactone and I could go on and on..
also when you use this method since the reaction goes to 100% na-ghb you get
more mileage(products) out of your lactone...

Also not using caustic chemicals eliminates alot of headaches and even if you
screw up the worst that would happen is a mixture of baking soda lactone and
water which is not very bad compared with swallowing a posion (which people
have done and been hospitalized for as seen in MM2K etc.)
Also good about this recipe is that you know how much final grams of na-ghb
you're going to have you will better be able to determine dosing....... When
using an NaOH recipe results can vary due to the nature of the reaction and you
end up with batches of various potency etc.

It is also easier to measure the ingredients,baking soda is of high purity and
available for almost nothing at your local grocery store and you can easily
make a powdered ghb simply by boiling the water away and letting dry...

Making NaGHB with baking soda and Lactone and water in a crock pot....
The only real problem with this recipe is that it takes time for it to happen,
the reaction happens gradually thus allowing all the reactants to react if you
give it enough time thus leaving you with no traces of lactone etc. the final
product will smell like water and the taste will be nicer then your used to if
your used to g made with NaOH...If all you have is lactone and you wanted some
right away you could make some with NaOH, then use what you'd like then dump
that mix into a crock pot add some baking soda and get the rest of the lactone
to react and purify/clean your g mix up...(note: SWIM has yet to do that,
though his plan might be to make some G with KOH and make some NAGHB with
baking soda then add the K-GHB to crockpot add additional baking soda to react
with lactone in the KGHB and have a k/Na g mixture without any
lactone/impurities)..

The recipe is very simple..and a crock pot can be bought from walmart for
$9.99...

1 part GBL
1 part Baking soda
2 parts water
(example: 250g GBL,250g arm+hammer,500mL H2O)

(trivia: sodium bicarbonate is 84g's per mole and butyrolactone is 86g's per
mole, thus the above combination will give you a slight excess of baking soda
thus making sure all the GBL reacts, if you put say only .9 parts Baking soda
for 1 part GBL then you'd have some left over unreacted lactone.. not good! you
might want to put in a few extra grams baking soda just to be double sure...)
dump ingredients together into the crock pot...turn the crockpot on low heat,

you must cover the crock pot with a bowl and then fill that bowl up with water,
this will keep the lid cool and let the lactone drip back down into the
solution so you don't waste lactone by boiling it off, if anyone wants a little
picture or diagram of this let me know! It's really simple just put a big
ceramic bowl from your cabinet on the top of the crockpot acting as your lid
and pour water into the bowl..(the water will slowly boil away and you should
add more to the bowl whenever you get a chance, if you come home and find the
bowl empty NBD just fill it back up and everything should still be fine,
perhaps a tiny bit or reactants/product may have escaped but probably not much
and very possibly none at all)

You then leave this crockpot on LOW heat for 36 hours and all the reactants
will go thru to final product...SWIM likes to leave it go for an extra day or
two so you definetly have a product containing no lactone and everything gets
reacted etc. Most of the stuff will react in about 18 hours , so if you wanted
to steal a little from the pot then let the rest keep reacting to completion
then you should wait a day or so after starting before doing so...

Much credit goes out to c6h10n2o2 who originally designed and formulated the
recipe. If anyone has any questions or if there is enough interest I will put
it up on a/my website...maybe even make a diagram/illustration and extensive
commentary...of course if the lycaeum is interested in hosting such a page as
well, I'd be Honored if murple or someone at the lycaeum or erowid put it up!!
Click to expand...

- from the ghb newsgroup, the last time I let it react to.. ph 10-11 or so, then I just tossed some baking soda in there (a jar) and let it just sit on a heating thing for a long time. Well, ph about neutral, fine, thing is,

It honestly, doesn't even hardly taste SALTY anymore! I can mix 3g's of this GHB in a cup of water (small cup) and barely taste it.. where before with only using NaOH, there would always be a salty taste or something I can taste (I guess unreacted GBL??), why would baking soda let it react completely but it wouldn't otherwise with NaOH?
 
I always dry finished Na-GHB by pouring it out on tin foil and drying on the air-vent above my gas cooker, it gets pretty damn hot, and keeping the grill flame down low, I can evaporate it to powder consistency, I store the finished product as powder in a dessicator over NaOH.

The reason for the slight excess, is I ALREADY have a batch, with more GBL than I am willing to waste, that has some NaOH contamination, and it is slightly brown, I will probably try slightly acidifying the GHB in solution, on a small amount first, and taking it up in butane or ether for evaporation.

One thing I might try, for producing REALLY pure GHB, is first to reflux barium hydroxide with GBL, to form the barium salt, treatment of that with dilute H2SO4, should precipitate the extremely insoluable BaSO4, and leaves the free
gamma-hydroxybutyric acid in solution, which would be filtered clean of residual BaSO4, then added dropwise to a saturated solution of sodium bicarbonate, using CO2 evolution to determine when perfect neutralisation had occurred.
 
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That's a really unbelievably complex procedure when you could just simply heat gbl with a concentrated solution of baking soda in water and get what you want. It may take more time than the procedure you stated, but still it'll be a lot easier, and you won't have to worry about ingesting barium salts or your material spontaneously ring closing when you acidify it.
 
^ Barium is incredibly toxic, in case you didn't know. Most barium salts are S1 poisons - not something you want anywhere near your digestive system
 
I know Ba salts are toxic, my reasoning was, the sulfate, would be entirely insoluable, BaSO4 is used orally and up the arse in hospitals, is it not? to show up soft tissue on an x-ray scan?

Either way, fuck it, I just don't want to trash a whole arseload of GHB.
 
can any tell me what an NP slvent is? is it just a paint stripper/remover ect... plz get bk t me on this... thx
 
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