反应详情

1 g of t-butyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate in 50 ml of toluene is treated with 0.82 g of 2,4-bis(p-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulphide and the mixture obtained is heated to boiling under reflux for 6 hours. The mixture is poured into water and the toluene phase is separated. After drying the organic phase over magnesium sulphate and evaporation, the crude product is chromatographed on silica gel. There is obtained t-butyl 5,6-dihydro-5-methyl-6-thioxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate on melting point 207°-208°.

1. customthe mixture obtained
2. temperatureis heated
3. temperatureunder reflux for 6 hours
4. customthe toluene phase is separated
5. customAfter drying the organic phase
6. customover magnesium sulphate and evaporation
7. customthe crude product is chromatographed on silica gel