I should probably start out by saying: pressurized reactions are generally not a good idea. Why try to make a bomb if you can just put a condenser on top? Right. Still, trying things is not illegal (actually that depends), and in my case I am starting out from 0.15g pseudo, keep it all very small and check pressure at certain times in the vial. According to some calculations, I should be safe either way with this minimal amount of material, the vial itself is tested for 160 psi and probably more (always check for cracks).
I cleaned my pseudo with cation exchange + base extraction. I'm not completely sure about its purity but I have to guess it is mostly pseudo freebase. Piss poor yield btw (20%). I still have the remains. I will use freebase for the reduction.
My first reaction: 0.15 PSE freebase / 0.05 redP / 0.3 I2/ 0.3 ml dH20. 120 °C (in flask), 24 h. I used a stirring bar with the result that a lot of RP was stuck to the glass at the end, so not sure how good that interaction was. There is reflux in the flask as the top of the vessel isn't cooled. Added water -> all yelow -> filter RP--> added base to filtrate + some thiosulfate + toluene and extract toluene and let it evaporate. Very little oily substance was detected, maybe a few mg. Tested this and it was a pretty harsh, corrosive smoke; it was meth. But not anywhere close to an acceptable yield. I did more pulls; close to nothing... I evaporated the water: nothing left (apart from the KOH/salt obviously but nothing of any use. So the PSE/meth got away from me (or was it just not pure at all?). I'm also thinking, did I fuck up with evporating the toluene with the meth freebase? Could it have been evaporated with the toluene. I was thinking it is unlikely but not impossible...
Second try: I took more care now, 0.15g PSE freebase/ 50 mg RP / 0.3 I2/ 0.3 dH2O. But I let the RP and I2 react first (these are pure). A brown mixture was formed (I was thinking, if the pressure reduces HI formation I might need to do that first (although I don't really believe in this myself). After 1 h I added 0.03g RP extra. The reaction is mostly yellowish and the RP is clumped together, still fizzling though and seems to increase with added RP. Let is stand for 24 h (120°C always) and it is still fizzling, decided to leave it 12 more hours (still bubbles forming on the RP). If I remove the cap, some more fizzling is occuring, also some white smoke, but no real pressure release from opening the vial. I decide to stop the reaction. Add water, but this time the mixture looks milky white... Thats no good. I do the whole process, add base --> now it gets very cloudy, some fluffy stuff is forming (so my PSE isn't as pure as I was thinking?). I try to take a picture. In an act of God my cat makes an entrance (she is not allowed in this area and is of the intelligent kind so she knows this, but unfortunatly she also has good stealth). Tipped the whole thing on the floor. Added some extra brine to the solution on the floor with my tears. Try to recuperate some in the most sad of scenes. What I have left is now a brown water suspension with a clear toluene layer (and a good looking floor cleaned by KOH). I decide to make extract the toluene and add HCl (didn't like my freebase results and maybe with the smallest yield at least cystals will have some volume visually). Of course, I have little hope at this point. I put a fan on the aq Hcl solution and little heat (outside). This is happening as I type so little cliffhanger here.
Some thought:
-I will have to extra clean my pseudo, I guess. The milky appearance after I add water in the second try annoys me. If I have meth HI or pseudo HI, they should dissolve in water so something is happening that I don't want. Also, this didn't happen with shorter times. Is there a possible side reaction that forms a compound not easily dissolved in water?
-don't have too much idea if the pressure vessel is working against me here. I still had bubbles forming way beyond 24h, but not sure if I have to read too much into that
-I'm thinking of adding less water still. In a reflux setup with a cooler you will have more water losses compared to a pressurized vessel. Of course, the whole reaction is never really boiling as the pressure is presumably preventing this. In my simple mind, I don't need the boiling, I just need the temperature to proceed with the reduction.
Tips welcome;