Has anybody tried this procedure? I have been planning using the products for this in a nice Strike inspired performic acid oxidation to the lovely ketone.
" A solution of 110 g of catechol, 120 ml of 50% aqueous sodium hydroxide and 200 ml of DMSO was heated to 98°C and stirred at that temperature for 30 minutes. This solution at 98°C. was added over a 30 minute period to a refluxing solution of 120 ml of methylene dichloride in 300 ml of DMSO. Thereafter, the reaction mixture was stirred at reflux for 1.5 hours. Steam was then passed into the mixture to achieve steam distillation of the product. The distillate (600 ml) was extracted with 100 ml of methylene dichloride, which extract was washed once with 50 ml of water. The methylene dichloride solution was then concentrated in vacuo at 40°C to yield 119.4g of a colorless oil. Gas chromatographic analysis showed 97.5% methylenedioxybenzene. Yield 116.4g (95.4%)."
It looks far faaarrrr too easy and OTC to be the real deal, instead of passing steam into the flask surely you could flood the flask with water and steam distill that way?
Thoughts?
" A solution of 110 g of catechol, 120 ml of 50% aqueous sodium hydroxide and 200 ml of DMSO was heated to 98°C and stirred at that temperature for 30 minutes. This solution at 98°C. was added over a 30 minute period to a refluxing solution of 120 ml of methylene dichloride in 300 ml of DMSO. Thereafter, the reaction mixture was stirred at reflux for 1.5 hours. Steam was then passed into the mixture to achieve steam distillation of the product. The distillate (600 ml) was extracted with 100 ml of methylene dichloride, which extract was washed once with 50 ml of water. The methylene dichloride solution was then concentrated in vacuo at 40°C to yield 119.4g of a colorless oil. Gas chromatographic analysis showed 97.5% methylenedioxybenzene. Yield 116.4g (95.4%)."
It looks far faaarrrr too easy and OTC to be the real deal, instead of passing steam into the flask surely you could flood the flask with water and steam distill that way?
Thoughts?