反应详情

A solution of 8-fluoro-3-methyl-4,5-dihydro-1H-benzo[b][1,4]diazepin-2(3H)-one (6.2 g, 32 mmol) and Lawesson's reagent (25.9 g, 64 mmol) in tetrahydrofuran (300 mL) was heated at 80° C. for 1 hour. 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 8-fluoro-3-methyl-4,5-dihydro-1H-benzo[b][1,4]diazepine-2(3H)-thione as a pale green solid (10.0 g, crude).

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)