반응 #3683

반응 방정식

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

용매

dichloromethane

반응 조건

후처리

1. 1
   세척The mixture is washed with H2 O, 1N HCl, H2O, 1M NaHCO3, brine
2. 2
   건조dried (Na2SO4)
3. 3
   세척the filter cake washed with dichloromethane
4. 4
   농축The filtrate is concentrated
5. 5
   기타the solid crystallized from ethyl acetate
6. 6
   기타to give crystals, m.p. 137°-140° C.

실험 절차

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.

출처