반응 #449605

반응 방정식

6,11-dihydro-5H-dibenz[b,e]azepine

N,N-diisopropylethylamine

4-[(2-methyl-3-fluorobenzoyl)amino]-3-chlorobenzoyl chloride

→

desired product

수율 72.1%

N-[4-[(6,11-Dihydro-5H-dibenz[b,e]azepin-5-yl)carbonyl]-2-chlorophenyl]-2-methyl-3-fluorobenzamide

수율 72.1%

용매

methylene chloride

반응 조건

후처리

1. 1
   세척The reaction mixture is washed with water, saturated NaHCO3
2. 2
   건조dried (Na2SO4)
3. 3
   workup.ADDITIONHexane is added to the filtrate at the boil

실험 절차

A mixture of 1.0 g of 6,11-dihydro-5H-dibenz[b,e]azepine, 0.80 g of N,N-diisopropylethylamine and 2.01 g of 4-[(2-methyl-3-fluorobenzoyl)amino]-3-chlorobenzoyl chloride in 100 ml of methylene chloride is stirred at room temperature for 18 hours. The reaction mixture is washed with water, saturated NaHCO3, dried (Na2SO4) and passed through a pad of hydrous magnesium silicate. Hexane is added to the filtrate at the boil to give 1.79 g of the desired product as a crystalline solid, m.p. 254°-256° C.

출처