反应详情

A solution of 7-bromo-4,5-dihydrospiro[benzo[b][1,4]diazepine-3,1′-cyclopropan]-2(1H)-one (267 mg, 1.0 mmol) and Lawesson's reagent (606 mg, 1.5 mmol) in tetrahydrofuran (15 mL) was heated to 80° C., and maintained at the same temperature for 1 hours. The mixture was concentrated. To the residue was added water (50 mL), extracted with ethyl acetate (50 mL). The organic phase was washed with water (50 mL*2), dried by sodium sulfate, filtered and concentrated to give a residue. The residue was purified by column chromatography (silica gel, petroleum ether/ethyl acetate=6:1) to afford 7-bromo-4,5-dihydrospiro[benzo[b][1,4]diazepine-3,1′-cyclopropane]-2(1H)-thione (125 mg, 44%).

1. temperaturemaintained at the same temperature for 1 hours
2. concentrationThe mixture was concentrated
3. additionTo the residue was added water (50 mL)
4. extractionextracted with ethyl acetate (50 mL)
5. washThe organic phase was washed with water (50 mL*2)
6. dry with materialdried by sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customto give a residue
10. customThe residue was purified by column chromatography (silica gel, petroleum ether/ethyl acetate=6:1)