反应详情

A mixture of 0.185 g of 5,10-dihydro-4H-pyrazolo[5,1-c][1,4]benzodiazepine, 0.391 g of 4-[(5-fluoro-2-methylbenzoyl)amino]-2-chlorobenzoyl chloride and 0.158 g of diisopropylethylamine in 10 ml of dichloromethane is stirred at room temperature overnight. The mixture is washed with H2O, 1 N HCl, H2O, 1M NAHCO3, brine and dried (Na2SO4). The solution is passed through a thin pad of hydrous magnesium silicate and the filter cake washed with dichloromethane. The filtrate is again passed through a thin pad of hydrous magnesium silicate. The filtrate is concentrated and the solid crystallized from ethyl acetate to give crystals, m.p. 137-140° C.

1. washThe mixture is washed with H2O, 1 N HCl, H2O, 1M NAHCO3, brine
2. dry with materialdried (Na2SO4)
3. washthe filter cake washed with dichloromethane
4. concentrationThe filtrate is concentrated
5. customthe solid crystallized from ethyl acetate
6. customto give crystals, m.p. 137-140° C.