反应详情

A mixture of 0.5 g (0.00155 mole) of 5-(2-chlorophenyl)-1,3-dihydro-7,8-difluoro-2H-1,4-benzodiazepin-2-thione (IImm), 10 mL of ethanol and 0.62 g of 60% sodium hydride was heated at reflux for 24 hours. The mixture was cooled, diluted with ethyl acetate and washed successively with water and then brine. The ethyl acetate extract was dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to give 0.52 g of 5-(2-chlorophenyl)-1,3-dihydro-8-ethoxy-7-fluoro-2H-1,4-benzodiazepin-2-thione (IIg) as a yellow solid. MH+/Z=349.

1. temperaturewas heated
2. temperatureat reflux for 24 hours
3. temperatureThe mixture was cooled
4. washwashed successively with water
5. extractionThe ethyl acetate extract
6. dry with materialwas dried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure