For what it is worth:
"25.5g of crude anethole epoxide was removed from the freezer and placed in a simple distillation unit that utilized a sand bath to provide heat. Stirring and heating to 200°C commenced. After about three hours and numerous cranks of the heating dial, nothing had distilled across so the bee went "insulation crazy". More sand was added to the bath and the still head was wrapped in rockwool. After about three more hours and numerous more cranks on the heating dial nothing had distilled across. The max temp had been reached on the hotplate, so the whole unit was shut down and allowed to cool. After cooling the bee expected to find a charred black mess in the distillation flask, but instead found that the red/gold epoxide had turned into an opaque black liquid.
The sand bath was replaced with an oil bath and vacuum distillation was commenced. The first fraction to come across was a mobile brown oil (ketone!) with the exact properties described elsewhere by Chromic. 9.3 grams of ketone, bisulfite tests confirmed this. The next fraction came across about 14° higher and was a pale yellow oil, similar in smell to the original epoxide, 2.9 grams that was assumed to be the glycol. (How does one test this?)
The remaining contents of the flask would not distill across at higher temps. This is primarily because of the fact that upon cooling, the distillation flask contents turned into a thick, black tar. Clean up was achieved by soaking in acetone and using conc. sulfuric to clean up the remainder. The magnetic stir bar used was toast.
Amination of the ketone was not attempted."
BB 7.0
