反応 #3671

反応方程式

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

溶媒

methylene chloride

methylene chloride

反応条件

後処理

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

実験手順

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.

出典