反应详情

A solution of 4.6 g of 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine in 100 ml of dichloromethane was stirred under ice-cooling and 5.2 g of m-chloroperbenzoic acid was added. The mixture was further stirred for 40 minutes, after which it was washed with a solution of sodium sulfite, a saturated solution of sodium hydrogen carbonate and water in the order mentioned, and followed by drying over Na2SO4. The solvent was then evaporated off and the crystalline residue was collected by filtration and washed with ethyl ether. The above procedure provided 3-methylsulfinyl-11H-s-triazolo[3,4-b][3]benzazepine as crystals. Recrystallization from methanol yielded colorless needles melting at 176°-177° C.

1. temperaturecooling
2. washafter which it was washed with a solution of sodium sulfite
3. dry with materialby drying over Na2SO4
4. customThe solvent was then evaporated off
5. filtrationthe crystalline residue was collected by filtration
6. washwashed with ethyl ether