Ok I dug this out from the Nook
This is the only info that is near complete that I have found.
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any alkaline extraction will leave you with only cathine and crap.
it has to be an acidic extraction. blend fresh herb with water and ice to a smoothie. put in beaker and add some HCl and stir (to convert the alkaloid organic salts to the hydrochloride). keep agitating until the ice has melted and the soup is pretty much liquid. Strain through cloth then vac filter (diatoms or celite can help if it gets too gluggy). if your soup is likely to get much above 0 degC then stick it in the freezer for a little while. Also put any finished filtrate into the freezer.
Once all of it is done, chill to -10 or lower. Prepare a 5% solution of NaOH and chill to -10.
Now comes the part where you have to be VERY quick. Anything more than 15 minutes between now and when you add the acid and I doubt you would get ANY product.
Add as much NaOH solution as needed to bring filtrate to pH 13. Quickly extract with suitable solvent (note: years ago when I tried this I used ether, which worked extremely well for several reasons. This is simply not readily available anymore. DCM would work from a solubility aspect, but may cause emulsion. Naptha would work, but requires large volumes, Xylene I have no idea, but it's a good bet.)
Once you have all your freebase in solvent, make sure to give it a couple of washes. If you use ether you can now add HCl until pH4 and evaporate the solvent by dipping in hot water bath and blowing air into the top of beaker. Note that the 15 minutes counts to the point where you add the acid!
If using naptha etc you simply add HCl to ph3, then add equal amount (compared with HCl) of water. Separate water layer, extract again with just water, combine water layers. Put a 2mm layer of the water layer in pyrex dish, set up fan to evap solvent residues, then use heatgun or blowheater to direct hot airstream over dish while agitating the material with plastic spatula. Eventually it will crystalise.
Both methods result in a highly acidic hygroscopic mass of crystals or goop which needs to be kept dry.
Once dry simply add enough acetone to cover the crystals in a beaker (or more if it is really dirty), heat acetone to boiling point in hot water bath, let cool for 1 minute, put beaker in sealed zip bag and stick in freezer for 1 hour (depends on volume - contents must get to -5). Vac filter in mini buchner.
You still keen on doing it? Sadly it is illegal now where I am. Let me know how you go, cos so far only one person has been able to copy this successfully.
