反应详情

温度

70 °C

A suspension of P4S10 (36.1 g, 81.1 mmol) and Na2CO3 (8.6 g, 81.1 mmol) in 1,2-DCE (700 mL) at room temperature was stirred for 2 h before Methyl[(3S)-5-(4-chlorophenyl)-7-(methyloxy)-2-oxo-2,3-dihydro-1H-1,4-benzodiazepin-3-yl]acetate (for a preparation see Reference compound D) (16.8 g, 45.1 mmol) was added. The resulting mixture was stirred at 70° C. for 2 h before being cooled and filtered. The solid was washed twice with DCM and the filtrate washed with sat. NaHCO3 and brine. The organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure. The crude product was purified by flash-chromatography on silica gel (DCM/MeOH: 99/1) to afford the title compound (17.2 g, 98% yield) as a yellowish solid. LC/MS (Method A): m/z 389 [M(35Cl)+H]+, Rt 2.64 min HRMS (M+H)+ calculated for C19H1835ClN2O3S 389.0727. found 389.0714.

1. additionwas added
2. temperaturebefore being cooled
3. filtrationfiltered
4. washThe solid was washed twice with DCM
5. washthe filtrate washed with sat. NaHCO3 and brine
6. dry with materialThe organic layer was dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customThe crude product was purified by flash-chromatography on silica gel (DCM/MeOH: 99/1)