反应详情

A solution of 8-fluoro-3-methyl-4,5-dihydro-1H-benzo[b][1,4]diazepine-2(3H)-thione (5.0 g, 23.8 mmol) and acetohydrazide (2.64 g, 35.7 mmol) in n-butanol (60 mL) was heated at 130° C. for 15 hours. The mixture was concentrated in vacuo, and the residue was purified by column chromatography (silica gel, petroleum ether/ethyl acetate=5:1-2:1) to afford 4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine, 5,6-dihydro-1,4-dimethyl-9-fluoro-as an off-white solid (1.9 g, 34%). LRMS (M+H)+: calcd 232.11. found 232.

1. concentrationThe mixture was concentrated in vacuo
2. customthe residue was purified by column chromatography (silica gel, petroleum ether/ethyl acetate=5:1-2:1)