反应详情

A solution of 1-(4-chlorophenyl)-1H-benzo[b][1,4]diazepine-2,4(3H,5H)-dione (2.00 g, 7.0 mmol) and P2S5 (1.87 g, 8.4 mmol) in pyridine (40 ml) was refluxed, with stirring for 1 h under N2 atmosphere. The solvent was evaporated in vacuo to afford a residue. The residue was purified by column chromatography (silica-gel, DCM:MEOH=40:1) to give 1-(4-chlorophenyl)-4-thioxo-4,5-dihydro-1H-benzo[b][1,4]diazepin-2(3H)-one (1.05 g, 49%). LRMS (M+H+) m/z: calcd 302.03. found 302.

1. customThe solvent was evaporated in vacuo
2. customto afford a residue
3. customThe residue was purified by column chromatography (silica-gel, DCM:MEOH=40:1)