反应详情

A solution of diazomethane in ether was added to a suspension of 6 g (0.0163 mole) of 7-chloro-5-(2-fluorophenyl)-N-hydroxy-α-nitro-3H-1,4-benzodiazepine-2-methanimine in 100 ml of tetrahydrofuran. After sitting at room temperature for 1 hr the excess diazomethane was destroyed by addition of glacial acetic acid. The solvent was evaporated under reduced pressure and the residue was passed over 100 g of silica gel using methylene chloride. Crystallization from ether/hexane gave light yellow crystals with mp 130°-133° C.

1. customthe excess diazomethane was destroyed by addition of glacial acetic acid
2. customThe solvent was evaporated under reduced pressure
3. customCrystallization from ether/hexane
4. customgave light yellow crystals with mp 130°-133° C.