反应 #1546739

反应方程式

5,10-dihydro-4H-pyrazolo[5,1-c][1,4]benzodiazepine

4-[(5-fluoro-2-methylbenzoyl)amino]-2-chlorobenzoyl chloride

diisopropylethylamine

→

N-[4-(4H-Pyrazolo[5,1-c][1,4]benzodiazepin-5(10H)-ylcarbonyl)-3-chlorophenyl]-5-fluoro-2-methylbenzamide

溶剂

dichloromethane

反应条件

后处理

1. 1
   洗涤The mixture is washed with H2 O, 1N HCl, H2O, 1M NaHCO3, brine
2. 2
   干燥dried (Na2SO4)
3. 3
   洗涤the filter cake washed with dichloromethane
4. 4
   浓缩The filtrate is concentrated
5. 5
   其他the solid crystallized from ethyl acetate
6. 6
   其他to give crystals, m.p. 137°-140° C.

实验过程

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 H2 O, 1N 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.

来源