تفاعل #3683

معادلة التفاعل

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

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   غسيلThe mixture is washed with H2 O, 1N HCl, H2O, 1M NaHCO3, brine
2. 2
   تجفيفdried (Na2SO4)
3. 3
   غسيلthe filter cake washed with dichloromethane
4. 4
   تركيزThe filtrate is concentrated
5. 5
   أخرىthe solid crystallized from ethyl acetate
6. 6
   أخرىto give crystals, m.p. 137°-140° C.

الإجراء التجريبي

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.

المصدر