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Message-ID: <162353Z08031995@anon.penet.fi>
Newsgroups: alt.drugs
From: an121141@anon.penet.fi (Alice C. Livingston)
Date: Wed,  8 Mar 1995 16:20:43 UTC
Subject: GHB - a better described synthesis


This is an update from a post I made sometime last year.

Informational purposes only etc.

~~~

There has been a lot of talk about GHB on the net of late. I guess this is 
just adding to it but I will try to make sure all I mention is correct. 
Corrections welcome!

GHB or gamma-hydroxybutyrate is usually prepared in a form called sodium 
oxybate which is just the sodium salt of GHB hence its alternative name 
sodium gamma-hydroxybutyrate. Just to make things more complicated CAS 
refers to this salt as butanoic acid, 4-hydroxy, monosodium salt. In the 
earlier abstracts butyric replaces butanoic.

GHB is listed in Merk Ed. 11,8603 under Sodium Oxybate.

Enough of the naming mess, lets have a look at the stucture.

HO-(CH2)3-COOH

This is GHB. For the sodium salt replace the right most H with a Na. 
Pretty simple huh?

The precursor to sodium oxybate is called butyrolactone or 
gamma-hydroxybutyric acid lactone. It is fairly readily available (at 
least where Alice comes from) and not overly expensive. I would estimate
US$20 for 100 ml.

It is supposedly an excellent electrolyte for batteries and capacitors and
is used as an intermediate for numerous compounds. See Merk Ed. 11,1596 for
more information.


Here is what she looks like.

                      O
                     / \
                  H2C   C==O 
                    |   |
                  H2C---C2H

It should be apparent that opening this ring and a dash of NaO will yield 
Na-GHB. Easy? Most certainly. NaOH will open the ring and at the same 
time makes our salt and also some H2. [Erowid Note: The
Rhodium GHB Synthesis FAQ disputes the claim that Hydrogen is released 
by this reaction and we believe Rhodium is correct and this claim is in error. 
(Note Added June 26, 2008, thanks Jop)]

Two pieces of magic for the price of one.

Anyone interested in the mechanism behind the ring opening should be aware 
that the butyrolactone is saponified - any organic chem text will give 
more information.

Below is what an hour browsing the Chemical Abstracts yielded.

J.Am.Chem.Soc 51,260 (1929) refluxes NaOH and butyrolactone in water for a 
few hours and the resulting yield is poor, though the procedure is simple 
and therefore probably favoured by some. Summary follows.

16.3g butyrolactone and 7.4g NaOH were disolved in 30cc. of water and 
bolied under reflux for three hours. AT the end of this time more water 
was added to disolve the salt and the solution was filtered and 
evapourated to dryness under reduced pressure. The salt was recrystalised 
from alchol. Yield was 11.5g.

CA 107:6774e is better but more difficult method. Summary follows.

15.7g NaOH in 1280 ml MeOH was added to 344g gamma-butyrolactone over 1-
1.5h at 40C under an inert CO2 free atmosphere. After stiffing for 3h, 
220g of product was collected.

CA 107:39210w is another patent from by the same people as above. It 
effectively states the same thing but that the rate of addition was 
controlled to maintain a potential of 700mV to prevent the introduction of 
a carbonate. Raises more questions than it answers.

CA 59:11234e would be my procedure of choice though Alice is somewhat suspect 
of their yields. Summary follows.

To a hot solution of 225ml rectified EtOH, 45ml H2O and 220g NaOH, 489g 
gamma-butyrolactone was slowly added and the mixture kept boling for 30 
min. The ppt. crystalised from EtOH yielded 560g Na-gamma-hydroxybutyrate.

Here is how Alice applied the above...

To a round bottomed flask suspended in a bath of candle wax heated by an
electric hotplate was placed 10 ml EtOH, 4ml H2O (15ml 80% alc/vol Vodka
should substitute okay for these two) with about 10g NaOH.

The weighing of NaOH was done without an accurate scale and was probably 
over estimated. Using exactly 10g of NaOH will still mean that it is in
excess thus less should be okay - Alice used this amount to ensure all the
butyrolactone would be reacted.

It is probably unwise to use hardware store lye or whatever due to
possible impurities combined with the fact that relatively large amounts
of GHB which have to be ingested for an effective dose.

A condensor was placed on the flask and Alice waited till all was under
reflux. The NaOH did not completely disolve.

20 ml of butryolactone (M=86.09 g/mol; 1 litre=1.13 kg) was slowly added
over the next 15 minutes. By this time most of the NaOH had disolved.

The mixture was kept under reflux for the next 2 hours where upon the
condensor was removed and the EtOH and much of the water was allowed to
boil off - this took place over a period of an hour or so. Good ventilation
is a must at this point.

A white, thick oil remained which was quickly poured out onto a flat surface
and rapidly solidified into a white waxy solid about 5mm thick.

This solid was rather basic due to Alice's excess usage of NaOH so it was
roughly weighed, then placed in about 200 ml of hot water in which is disolved
easily. With the aid of litmus paper (remember blue equals basic) HCl was
added till the solution was slightly acidic.

HCl is the ideal acid to add as NaOH + Cl -> H2O + NaCl; that is salty
water (ugh).

Checking the pH of your product is of the uppermost importance. It must be
fairly neutral before you even contemplate ingesting your Na-GHB. Or to
put it another way - if you are really going to fuck up and hurt someone,
having an overly acidic or basic product is how you will do it.

Alice calculated the volume needed to drink for 1.5g of Na-GHB, consumed it
grinning and bearing the intense salty taste (this is due to the NaCl,
Na-GHB is pretty much tasteless when pure) sat, waited for 5 minutes and
never looked at alcohol again :-)

All good fairy tales have a happy ending and this is no exception, being
no longer dependent on alcohol is a delight, better than any prince or
princess!

A second time Alice essentially followed the above procedure but used less
NaOH. The final product was neutral but with some oily liquid which did
not solidify which was assumed to be unreacted butyrolactone which was
poured off ready to be used some other time.

This product was essentially taste free.

Butyrolactone an LD50 of 1.5g/kg in rats, better than that of GHB itself
so it should not be of too much concern, though Alice has corresponded
with a person who suspected that this impurity may be the cause of very
slight headaches which some consumers suffered from the next morning. 

A standard dose of GHB is rather hard to determine. Net information 
mentions 'half a teaspoon'. Medline seems to indicate that an effective 
dose varies greatly from person to person.

Medical use in the treatment of narcolepsy and alcohol withdrawl is almost 
invariably 50 mg/Kg per day. It is probably safe to assume this is a safe 
starting dose.

Reports mention overdosage can result in 'coma and seizurelike activity'. 
The mentioned amounts which caused these problems were from .25 of a 
teaspoon to 4 tablespoons. Full recovery seems to be universal.

This further goes to show that each persons reaction is very individual.

For more information on the qualitative effects of GHB, see
[Ed Note: Erowid.org/chemicals/ghb/].

Of particular interest here is a posting by rich@weeds.xs4all.nl from the
smart-p mailing list which gives an excellent description of the history,
pharmacology and recreational used of GHB. It is a must-read before you
experiment with the chemical.

Also there is a posting by dk104@cleveland.freenet.edu which is supposedly
a post for a friend, 'Frank', who describes how he combatted alcohol abuse
with GHB and seemingly won.

Alice understand that the author of this post's name was not actually
'Frank' and that he was an alt.psychoactives regular who finally outed
himself as the actual author. If anyone know of his email address please
contact Alice at the anon email address attached.

Alice would appreciate hearing from anyone who has attempted any of the
above, be it tasting or cooking.

Slowly slip away, be careful and most of all have fun!

Love Alice Livingston.

~~~
Alice Livingston
'I am just a truck driver on the information superhighway'



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=============================================================================

From: an121141@anon.penet.fi (Alice C. Livingston)
Date: 1995/11/06
newsgroups: alt.drugs

Here are some corrections and safety tips which correspond to the ghb 
synthesis archived at [Erowid.org/chemicals/ghb/ghb_synthesis1.shtml]

Perhaps Lamont could update that version with the follow information. I 
will give the whole mess of a document a complete overhaul when I get 
the time.

Added notes are included in [braces like this]

~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

[...snip...]

It should be apparent that opening this ring and a dash of NaO will 
yield 
Na-GHB. Easy? Most certainly. NaOH will open the ring and at the same 
time makes our salt and also some H2.

Two pieces of magic for the price of one.

[well actually some magic and some fantasy as it turns out - no H2 is 
evolved]

[...snip...]

The weighing of NaOH was done without an accurate scale and was probably 
over estimated. Using exactly 10g of NaOH will still mean that it is in
excess thus less should be okay - Alice used this amount to ensure all 
the
butyrolactone would be reacted.

[use an accurate scale and use the ratios mentioned in the above chem 
abstract. By doing this you will not have to fiddle around with the pH 
at 
all]

[...]

A white, thick oil remained which was quickly poured out onto a flat 
surface
and rapidly solidified into a white waxy solid about 5mm thick.

[actually the oily substance is clear until it cools into a white solid]

[...]

A second time Alice essentially followed the above procedure but used 
less
NaOH. The final product was neutral but with some oily liquid which did
not solidify which was assumed to be unreacted butyrolactone which was
poured off ready to be used some other time.

Butyrolactone an LD50 of 1.5g/kg in rats, better than that of GHB itself
so it should not be of too much concern, though Alice has corresponded
with a person who suspected that this impurity may be the cause of very
slight headaches which some consumers suffered from the next morning. 

[butyrolactone is something you really do not want to injest at all. 
While the LD50 is fairly high there are unanswered questions about its 
long term toxicity. One method which may be successful in reducing the 
amount of unreacted butytolactone is to boil the final product at 204 C 
(butyrolactone's boiling point) until no more bubbles appear. You could 
also recrystalise the final product from alcohol] 

~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

Alice Livingston
'Still softly it floats away'