In the methylenation step, all procedures say to steam distill the product for purity. Is it OK for swim to do a regular distillation here (i.e., simple distillation to remove dihalomethane and solvent, then switch to a vacuum distillation to isolate the safrole)?
Also, SWIM has one last question about the demethylation procedure (the 3rd procedure on Rhod's page, by Startinout using AlI3)... this is a direct quote from Rhod's page:
the solid collected immersed in ethyl acetate, this is swirled for a couple of minutes, then filtered. The ethyl acetate is seperated from the water (collected through the filtration) and removed and what you have left is a tan coloured solid with a charactistic 'smoke' smell...
So, is the solid that SWIN immerses in the ethyl acetate the one he wants to keep? Or, when I remove the ethyl acetate will a new precipitate form? What exactly is meant by "remove the ethyl acetate?" SWIN thinks someone is going to have to spell it out for him. He thanks everybee in advance for help! peace