sublimation recrystallisation of pfed

loki · guinea pig

swil recently constructed a coldfinger condenser, ostensibly for purifying iodine, but he was thinking about whether this could be used for pseudoephedrine.

Being that the majority of pill constituents are lower boiling than ephedrine, swil thought maybe boiling the freebase pseudo it and crystallising it would work.

Here's how swil sees it happening

1. grind pills into powder
2. make up some sodium ethoxide with denatured ethanol and sodium hydroxide, and mix with pill mass in the bottom of the flask the coldfinger fits into with enough of the sodium ethoxide to make it into a slurry, mixing thoroughly, and then let it evaporate.
3. Rig up the coldfinger condenser in the flask, and heat the now dry basified pill mass.

Will the pseudoephedrine freebase boil out of this gunk and stick to the coldfinger? I can't see why not, being that pseudo does not degrade significantly from steam distillation.

IndoleAmine · Dreamreader Deluxe

With steam distillation, you have at most 100°C inside the vessel you are heating.

When heating a mixture of solid compounds, the temp. can go much higher very easily, and that's the problem - it chars and burns.

But I remember there was someone (Prepuce?) at the old hive who was looking into "SPD" (short-path distillation) of pseudoephedrine freebase lately, before our home went offline..

(maybe you should look for it in the archives - or ask Prepuce himself, I think he's around at WD sometimes..)

i_a

loki · guinea pig

i was just thinking it might be more sensible to extract the freebase with the alkalinised alcohol and then boil that out into toluene or something (higher bp obviously better) a small amount mind, don't wanna be evapping tolly for *too* long, and then evaporate it and do the sublimation on the residue. I guess i'm just describing a dry a/b to a certain extent.

regarding temperature control, isn't that easy? just adjust the heating apparatus to the right temperature? Charring is a serious question though, lactose is a common component of pill formulations and it would turn into a hard black tar.

edit: swil tested a pfed.sulphate pill recently, one which he suspected of containing an orange gak. When the pill mass was refluxed in alkaline ethanol, the colour of the orange gak became distinctly darker and more orange. swil is not quite sure what to do with this pile of orange-infested alkaline ethanol extract. He is thinking steam bath dry it and try the molecular distillation thing on it, but he's not sure. that orange gak is nasty, it's like plastic.

jackoozzi · specialist

I saw this posted at the hive just before it closed unfortunately i did not keep the thread just the picture but it went something like this

grind pills with calcium carbonate (i think) add ammonia hydroxide till damp, heat till ammonia smell is gone then add tetra till a slurry add toluene and heat again filter then dry toluene completely (must be completely dry or it causes problems)
now add the lot to the pictured device and heat to 340f (i think) when snow flakes appear in the bowl start vacuum use the vacuum to pull it across
It was stated that this works with 80% returns
If you have any more questions ask and i will see what i rember

methyl_ethyl · Riedel De Haen

I suggest consulting the search engine at www.wetdreams.ws . There is extensive discourse related to Short Path Distillation, along with the picture jackoozzi posted, amongst other depictions of said apparatus. Just throw SPD into the search engine and hopefully you will find what you are looking for, short path distillation might possibly bring up more hits than SPD, not sure.

much_love

methyl_ethyl

Radiumhero · Sat Aug 20, 2005 6:25 pm

Well i did that one unwillingly by putting my nice freshly extracted ether - wet
pseudo freebase on a hotplate ( thought it was only a little warm ) and went to get some beer to watch the neat xtals grow but wtf i came back and the fcken whole air in the kitchen was flittering because of tiny xtals flying around what was left in the porcelain bowl was light brown stuff -.-