反应 #3671

反应方程式

Water

4-[(2-methyl-5-fluorobenzoyl)amino]-2-chlorobenzoyl chloride

10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine

N,N-diisopropylethylamine

→

glass

N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)-3-chlorophenyl]-3-fluoro-2-methylbenzamide

溶剂

methylene chloride

methylene chloride

反应条件

后处理

1. 1
   温度While cooling in an ice bath
2. 2
   洗涤the separated organic layer washed with saturated sodium bicarbonate
3. 3
   干燥dried with Na2SO4
4. 4
   其他The methylene chloride is removed in vacuo

实验过程

To a solution of 1.50 g of 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine in 25 ml of methylene chloride is added 1.23 g of N,N-diisopropylethylamine. While cooling in an ice bath, a solution of 3.08 g of [4-[(2-methyl-5-fluorobenzoyl)amino]-2-chlorobenzoyl chloride in 50 ml of methylene chloride is added. The reaction mixture becomes homogeneous and is stirred at room temperature for 18 hours. Water is added and the separated organic layer washed with saturated sodium bicarbonate, dried with Na2SO4 and passed through a short pad of hydrous magnesium silicate two times. The methylene chloride is removed in vacuo to give 3.81 g of a glass. A sample is crystallized from ethyl acetate to give crystalline solid, m.p. 200°-205° C.

来源