After extraction the non-polar is gassed, then the freebase is vaporized and condensed back into a solid.
That comment will mislead six thousand newbees into disaster. How about filling in the missing between-the-lines comments so you don't confuse the new ones, or the old geezers like me, who have nothing to do with their hands these days but bitch at the keyboard... ;D Damn pill laws! I have to drive a couple of hours just to get enough pills to make it worth my time to try any new method. (Get ready folks, its headed your way before you know it.)
First, to post a link to a post, put it's number in brackets. Your post number is 513459, put that in square brackets to obtain Post 513459 (https://www.thevespiary.org/talk/index.php?topic=8126.msg51345900#msg51345900)
(Prepuce: "Gaks that hold amines", Stimulants).
Now, those annoying detergents are of the polyoxoethylene type, eh? It would be ideal to perform an acid hydrolysis to crack those ether groups, but I don't know the conditions required or whether it would harm the pfed.
So let's imagine that they boil really high, and leave them as-is. Say we follow the following imaginary procedure:
pills are ground up with ammonia water and sodium carbonate until it is a pasty, chalky sludge. Then, the mixture is gently evaporated to yield a hard greasy cake which is crushed up and distilled as prepuce describes. Hopefully good yield of pfed.
Something worth trying, I guess.
Best luck 8)
can't resist mentioning that he was astounded! by the yeild.
The most likely explanation for the improved yield is that the pseudo you reacted was much cleaner than you have been reacting before. Yield improves with the cleanliness of the feedstock under virtually any set of PIE reaction conditions.
Scotty, for some experimental results that suggest something about the activity of the yellow gak, see SWIP's post Post 515408 (https://www.thevespiary.org/talk/index.php?topic=7964.msg51540800#msg51540800)
(Prepuce: "Another data point", Stimulants). It appears that ammonia causes the yellow oil to sink to the bottom when mixed with xylene, releasing the pfed which was completely converted to freebase by the ammonia with maybe a little help from the NaCO3. Better to get the job done, he now believes, with ammonia only, but he's the NaCO3 will still be needed to absorb H2O and the gak. He agrees that there is no need to add additional water.
In his experience the creamy mix isn't a problem, and you can really see this with the white 60s. You can see the mass decrease when the xylene is added, as the pfed freebase goes into solution.
SWIP would dearly love to find a convenient way to pull the pfed from the xylene directly, but remember, it's freebase and soluable at that point. He's not interested in evaporating xylene and isn't aware of any other options at the moment. The only purpose served by the second A/B is to get freebase, since vaporization doesn't work well with the hcl salt.
He believes that it's possible, and of course highly UN-desirable, to squeeze water/gak/yellow oil from the pill mass if it's squeezed or subjected to other forces that could suck it loose. But as long as only ammonia is used for the basing and in sufficient quantity--NO NaOH!!!--that the yellow gak completely releases the pfed. SWIP wouldn't be getting 60% plus yeilds if that weren't the case.
SWIP tried what you are suggesting with the tetra trap a long time ago, and it failed because the pfed just wasn't coming out. Your method may be slightly different, though, so by all means give it a try.
SWIP also tried just grinding pills, basing and evapping the whole mess. You actually get some yeild, but it doesn't work well because of the H2O, which comes out when you start heating it. It also stands to reason that the procedure is going to work better on reletively clean pfed than it will for a sample that still contains all the gak.
PP
swim has read in this post the MP of pseudo FB is 118, but if swim left his FB at 118C will it vaporize and move over at this temp? if not what temp is needed?
Also, swim thinks that the whole ammonia think is a waste of time and that its just the short path distilling that does all the cleaning.
So wouldnt it be best if the pseudo could be taken from pills and turned into freebase in the easiest/shortest amounts of steps?
Why doesnt one just
- Pull pseudo with alky and evap
- Dissolve whats left in water
- Add a pre made basic water solution to this until FB appear
- Collect FB with Xylene and evap Xylene for FB
- Distill FB
Swim has been wanting to try this for about a week now, ive even got a thread showing swim distilling setup Post 518820 (https://www.thevespiary.org/talk/index.php?topic=8156.msg51882000#msg51882000)
(12cheman12: "Cleaning Freebase", Stimulants)