Реакция #3683

Уравнение реакции

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

Растворители

dichloromethane

Условия реакции

Обработка

1. 1
   ПромывкаThe mixture is washed with H2 O, 1N HCl, H2O, 1M NaHCO3, brine
2. 2
   Сушкаdried (Na2SO4)
3. 3
   Промывкаthe filter cake washed with dichloromethane
4. 4
   КонцентрированиеThe filtrate is concentrated
5. 5
   Другоеthe solid crystallized from ethyl acetate
6. 6
   Другоеto give crystals, m.p. 137°-140° C.

Методика

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.

Источник