Since our Chief bee wasn't satisfied with the purity of GHB made with above "cheap+easy" method, I thought "why not slightly modify it to give acceptable pure product"? Yields could be somewhat better, but the only hard-to-get chemical needed is THF - the "precursor" in this synth.
So here is the improved procedure:
30 ml THF and 30ml D
2O were mixed in a beaker and chilled to below 0° in a fridge. During the time needed to cool sufficiently, ~40 grams KMnO
4 were finely ground using a mortar (be careful with the dust). To the prechilled THF/water solution were then added about 4 grams of the permanganate powder. Everything was stirred with a thermometer, watching the temperature. As soon as it hit +7°C, the therm. was rinsed with a bit ice-cold acetone and the beaker put back into the fridge. Every now and then (every 30-45 min.) the mixture was stirred using the thermometer, taking care that the temp. didn't rise to significantly above 10°C (if this happened, some cold acetone was added in little squirts) and put back to cooling.
This was repeated until the reaction had a dark brown appearance and the temp. didn't climb notably higher when being removed from fridge. Then (when NO temp. rise could be seen anymore!), the next few grams of permanganate powder were added and the stirring/cooling/diluting was repeated as necessary (during the last few additions, the reaction became very viscous, so much acetone was added, along with some ~30ml water - end volume was ~200ml), until further additions of permanganate resulted in purple color that didn't fade to brown anymore (in total, adding 34g KMnO
4 took more than 14 hours..
). The solution was then allowed to sit some more 2 hours before it was diluted with 50ml EtOH, stirred and again let sit for 2 hours.
The formed MnO2 settled down overnight as a dark brownish solid and on top appeared a slightly milky, off-white solution (containing acetone, water, ethanol, butyrolactone and unreacted THF - in that order). Everything was vacuum filtered through a pad of celite, basified to pH 11 with 20% KOH-solution and the solvents distilled of under "slight" vacuum. the remainder was then acidified to pH 5 by adding H2SO
4 dropwise with good stirring, resulting in precipitation of a small amount of K
2SO
4. The lactone/GHB/water mixture (?) was then steam distilled, the distillate transferred to a 250ml two-necked RBF fitted with a dropping funnel and a reflux condenser and heated to heavy reflux. Next, 2ml of a 20% KOH-solution (I usually prepare standardized solutions of acids and lyes I often use, in this case 20% KOH was what was at hand, maybe other concentrations work better - dunno) was added dropwise via additon funnel and reflux was continued for 2-3 minutes before heat was removed. After having cooled down a bit, the solution was brought to pH 8 with more KOH and the water was evaporated. The hot concentrated solution was then poured into a pyrex bowl and the remaining water slowly evaporated w/careful heating until the GHB potassium salt crystallized (it did so on cooling, together with a small amount of KOH wich solidified too). The total amount of collected solids was 13.4 grams.
This was put in a (clean!) mortar, quickly ground (better don't do this but dissolve the salt directly: it gets real wet real quick when mechanical "crushing" is attempted) and dissolved in some D
2O, brought to pH 7.1 by adding some drops of 37% HCl and diluted to a volume of 30 ml with more d.H2O to give a concentration of roughly 0.48g/ml, along with some KCl (probably the best "cut", as K
+ ions are exactly what your body needs when you're on GHB
).
The so obtained product is a bit salty, but the purity is good enough for human consumption (unless you use impure chemicals of course) - at least I tested it several times until now, and nothing has happened to me yet...
(of course this testing was only done to evaluate the grade of purity and the possible negative effects caused by contaminants - as said, no such effects were observed until now, so there are most likely few enough present to not bother with them)
And remember, the only things you need are:
KOH, H
2SO
4, acetone, ethanol (NOT denatured alc!! better use vodka (or similar) if u can't get abs.EtOH), THF, KMnO
4, a beaker, a thermometer, complete dist. setup (preferably for vacuum dist., but a simple one should suffice), a fridge - and a LOT of patience! I think this is still cheap and easy enough to justify the title of this thread *lol* - good luck..
Greetz A
