反応 #3695

反応方程式

ethyl 10,11-dihydro-10-(4-amino-3-methylbenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxylate

N,N-diisopropylethylamine

2,4-dichlorobenzoyl chloride

→

solid

収率 55.4%

Ethyl 10-[4-[(2,4-dichlorobenzoyl)amino]-3-methylbenzoyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]-benzodiazepine-3-carboxylate

収率 55.4%

溶媒

methylene chloride

反応条件

後処理

1. 1
   洗浄washed with water, saturated NaHCO3
2. 2
   乾燥dried with Na2SO4
3. 3
   workup.ADDITIONHexane is added to the filtrate at the boil

実験手順

To a solution of 0.30 g of ethyl 10,11-dihydro-10-(4-amino-3-methylbenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxylate in 20 ml of methylene chloride is added 0.15 g of N,N-diisopropylethylamine and 0.24 g of 2,4-dichlorobenzoyl chloride. The reaction mixture is stirred at room temperature for 18 hours and washed with water, saturated NaHCO3 and dried with Na2SO4. The organic layer is passed through a pad of hydrous magnesium silicate. Hexane is added to the filtrate at the boil to give 0.24 g of solid, m.p. 174°-184° C.

出典