It`s not necessary to evaporate IPA, but the T of mixture must be raised to 60C.
If the all chemistry is pure, that possible too much of CuCl2 could have reacted with amine.
Can you describe the colour of the mixture when adding CuCl2?
GhostChemistthe moment i added the copper solution (i used CuSO4*5H2O) to the rm it turned dark grey. i added it slowly, and after the first few drops i turned on the heat. (there was also what looked like undissolved borohydride granules in the rm.)
as i continued to add it it didn't really change color, but the copper oxide sediment formed like in the video. because of my hotplate i couldn't get the temp above 62C, so i kept it at 62c for about 3 1/2 hours.
However, i did another synthesis where there weren't any granules in the rm, and i held the temp at 80c after the addition of the CuSO4*5H2O solution, and it still gave the same product at the very last stage.
there was a synth i did where the rm turned dark green upon addition of CuSO4*5H2O, and after a few more drops it turned dark orange.
with all the synths i've done, everything in this first stage has at least appeared to be consistent with the video.
i think with all the synths i've done so far, after the addition of the CuSO4*5H2O i have either left the rm as is with the copper oxide sitting at the bottom for a couple of days before i separate it, or i left the separated solutions with the 25% naoh solution in them sitting for 2 days. could this be a problem?
also something strange that happened was something precipitated in the 'main orange solution' after leaving it for a couple of days on it's own, whether it was left with the naoh solution after seperation, or just left for 2 days before seperation with the copper oxide at the bottom. (i don't think the solution derived from the copper oxide extraction had any precipitate).
maybe another potential problem is that when i recrystallized some my p2np i tried using sodium bicarbonate to purify it but i added too much (about the same amount of sodium bicarbonate as p2np. i added it in solution when the p2np was dissolved in a hot etoh solution. (i then put it in the freezer, filtered it when the p2np had precipitated, then did a standard re-crystallization by just dissolving it and precipitating it after freezing.) but maybe the sodium bicarbonate wasn't removed. a possibility is that maybe the sodium bicarbonate is present in the p2np i'm using.