OK, so SWIM tryes isomerizing for the 1st time. Tried the Cao/KOH method. Put 50g "purified" safrole in a rb flask, add 7.5g CaO and .5g KOH. RB flask in oil bath on hotplate, heated to first sign of gentle boiling w/ occasional stirring. Waited for it to really bubble, then let that run for about 15 min. (SWIMs thermometer broke, so don't presently have any temps to site)So what does SWIM get- the "dark translucent oil" that its supposed to be? No, result is a thick light tan emulsion. Book says unreacted salts can be removed by water wash. So SWIM figures "what the hell" and adds water. Now there is this big gooey mass that resebles a light tan brain. So SWIM is franticly trying to "save" the result of this mess. Pours as much as possible into a glass jar. Its still there. The rest is gooing up another piece of glassware. Added dEtOH to try to remove. Seems to work. After sitting overnight, 2 layers form. Top is yellowish alcohol (and some iso or reg. safrole?) bottom is more tan sludge. SWIM assumes that the EtOH layer can be decanted off, dH2O washed used to recover the oil. Maybe will try repeated alc. washings to get as much oil out of the sludge crap as possible.
Trial #2: added 25g of "straight from the bottle" sassy to 3.5g CaO and .25 g KOH in rb flask. Heated slowly to boiling then let it go for about 15 mins. This time, after cooling, there is CaO sludge mess in the bottom and nice translucent dark oil on top. Suitable to pipet off the top and distil, for later use, SWIM assumes.
So what went wrong in trial #1? SWIM assumes "purification" method for sassy oil. The method w/ acetic acid wash followed by EtOH and H2O washes was used. Assumably, some of the acetic got tied up in the whole thing. (NOW a point of interest here- SWIM puified sassy in 2 "lots". 1st time, the resulting oil was a very clear pale yellow, 2nd ime, it was left kinda hazy. Stupid ass SWIM didn't think and used a combo of both the hazy and clear stuff for the failed isomerization. New Bees- learm from thjs fuck up: if its supposed to be nice and clear, but it ain't, don't use it)
Experienced Bees: anyone run into this nightmare before? Is SWIM going in the right direction with rectifying the "tan brain mess"? Is there a better way to save the safrole or iso- that is tied up in it? Filtration? Distillation? That sassy is pretty dear, so hate for it to be a total loss.
