>1) has anybee actually done the rearrangement in toluene?
Read up on Scooby Doo's post in Novel Discourse (J.Org Chem 1984, 49, 1830-1832) Post 264135 (https://www.thevespiary.org/talk/index.php?topic=11605.msg26413500#msg26413500)
(Scooby_Doo: "Ref on Isosafrole to diol via electro", Novel Discourse). In that reference they use a conc. of 1g tosic acid to 100ml of benzene to do the rearrangement. I'm sure toluene could substitute as a solvent, and the concentration of the acid catalyst left the same but the concentration of the intermediate raised. (ie use 1g p-tosic acid, 100ml toluene, 100mmol processed alkene) I'm working on getting OTC p-tosic, but I keep running into little problems. My biggest problem right now is removing the aqueous phase from the mixture without a dean-stark trap... I get this nasty reaction mixture after reacting conc. h2so4 / toluene, but there's a not-viscous lightly colored phase, and a very viscous dark colored phase. Oh well, that's for another thread! :)
>the proc. sounds promissing, but then the H2SO4-way is known to be simple
No isolation is required for the p-tosic acid method either.
>4) all of ottos anise oil was solid in the fridge and he didn't consider to purify first.
>did you purify it this way (freezing) once? how is it like to do?
I have frozen the oil, but just for the fun of it, I didn't consider that method to purify it. Read up on safrole purification from sassafras. The gist is to put a small amount in the freezer, and you'll get a seed crystal. Chill the star anise down to just below the freezing point of anethole (ie 15C or so), then drop in the crystals. Wait a few hours for it to crystallize and pour off what doesn't freeze, thaw the oil, and repeat to purify.
However, I used vacuum distillation to purify my oil.
>5) otto has no idea about PMMA. he read some discussion and some bees tell that
>its very good. some tell that its crap or evil. what to do then, how to know...?
Try it out yourself. Keep your dosage low and don't expect much. :)