Fantasma4500 - 27-1-2019 at 09:21
appears this reaction may form an organic nitrite compound with a high boiling point, attempting to seperate the more desirable chemical by distilling
it off resulted in the nitrite compound being left, eventually drying out and selfigniting, decomposing to yield carbon, nitrogen dioxide and horrible
fumes
it may be ideal to first mix the gaba, nitrite and acid mix with alcohol, decant the liquid off, evaporate off at low temperature in a wide dish,
dissolve the high boiling solvent in ethanol or acetone and be done with it
Use Steam Distillation
random7 - 29-1-2019 at 10:13
Steam distillation takes a little longer but no worries about decomposition.
morganbw - 31-1-2019 at 16:54
That is a good safety warning.
I am not versed in that synth but I am respectful toward organic nitrites.
Amos - 31-1-2019 at 21:36
If you're really this insistent on getting high off GHB, you can probably avoid a disaster like this by extracting your reaction mixture with
dichloromethane, extracting the DCM extract with sodium bicarbonate or other basic solution, then washing the aqueous portion with more DCM and simply
evaporating the aqueous layer to yield an oxybate salt. If you're dead-set on distilling it, protonate the last bit of solution with acid and extract
once more with DCM before distilling. Not that you'll obtain any higher purity by distilling at this point.
Fantasma4500 - 1-2-2019 at 14:28
i found DCM extraction to be quite tedious, however as i proposed drying out the mixture at low temp (60*C) under ventilation (butyric acid, mind you)
resulted in a gooey mixture with a lot of liquid in it, dousing that with acetone formed 2 layers to my surprise, the solvent doesnt appear to be very
soluble in acetone, however it can be used to wash the solvent from the solid inorganic precipitates. the solvent supposedly has 1.7 viscosity, water
being 1-3(?) seems pretty viscious, as you'd expect from a solvent with a high boiling point.
i think throughout some 200mL of DCM i managed to produce barely 15mL of solvent, maybe make that 300mL as i did many extractions, quite frustrating
to avoid getting the water layer into the distillation when you dont got a seperatory funnel, distillation also goes quite slow without vacuum
filtration, i find this to take many hours compared to just tossing it on a flat glass pan ontop of a pot with warm water under some ventilation, also
recall reading somewhere near 50% of the solvent remained, magically -- in the distillation flask, this was then pulled out using steam distillation
(which, by my experience you want to pay a lot of attention to not running dry)
i think the sodium salt is quite stupid especially if you fancy health, water retention etc, potassium would be ideal for dealing with water
retention, calcium and/or magnesium also quite doable considering you can take quite large amounts of both.
as you may understand the crippled yields ive gotten with DCM extraction compared to what seems like 50mL gooey, or well on closer inspection, a gooey
layer now appearing to be nearly 100mL starting from 60g GABA.. thats quite a leap. to deal with a bit of butyric acid fumes and just throw that on a
glass plate? cant wait to go out and do society a favor pulling all that grafitti off the walls.