Reacción #3683

Ecuación de reacción

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

Disolventes

dichloromethane

Condiciones de reacción

Tratamiento posterior

1. 1
   LavadoThe mixture is washed with H2 O, 1N HCl, H2O, 1M NaHCO3, brine
2. 2
   Secadodried (Na2SO4)
3. 3
   Lavadothe filter cake washed with dichloromethane
4. 4
   ConcentraciónThe filtrate is concentrated
5. 5
   Otrothe solid crystallized from ethyl acetate
6. 6
   Otroto give crystals, m.p. 137°-140° C.

Procedimiento

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.

Fuente