反応 #527208

反応方程式

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

溶媒

dichloromethane

反応条件

後処理

1. 1
   洗浄The mixture is washed with H2O, 1N HCl, H2O, 1M NaHCO3, brine and dried Na2SO4)
2. 2
   洗浄the filter cake washed with dichloromethane
3. 3
   濃縮The filtrate is concentrated
4. 4
   その他the solid crystallized from ethyl acetate
5. 5
   その他to give crystals, m.p. 137°-140° C.

実験手順

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 H2O, 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.

出典