反应详情

A stream of hydrogen sulphide was conducted for 1/2 hr. through a solution of 4.4 g (0.0172 mol) of 8-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carbonitrile in 100 ml of pyridine and 1 ml of triethylamine. The dark green solution was left to stand for 64 hrs., then de-gassed with a stream of nitrogen and subsequently completely freed from the solvents. The residue was partitioned between dichloromethane/tetrahydrofuran and water, extracted, concentrated, stirred vigorously in ether and filtered off under suction. There were obtained 4.55 g (91%) of 8-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-thiocarboxamide as yellow crystals.

1. waitThe dark green solution was left
2. custom, then de-gassed with a stream of nitrogen
3. customThe residue was partitioned between dichloromethane/tetrahydrofuran and water
4. extractionextracted
5. concentrationconcentrated
6. filtrationfiltered off under suction