반응 #449529

반응 방정식

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

4-nitrobenzoyl chloride

N,N-diisopropylethylamine

→

crystals

수율 68.9%

2-Chloro-5-(4-nitrobenzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine

수율 68.9%

용매

dichloromethane

반응 조건

후처리

1. 1
   온도is refluxed for 18 hours
2. 2
   온도The mixture is cooled
3. 3
   세척washed with H2O, 1N HCl, 1M NaHCO3, brine
4. 4
   건조dried (Na2SO4)
5. 5
   여과The solution is filtered through a thin pad of hydrous magnesium silicate
6. 6
   세척the pad washed with dichloromethane
7. 7
   농축The filtrate is concentrated
8. 8
   기타the residue recrystallized from dichloromethane-hexane

실험 절차

A mixture of 2.05 g of 2-chloro-6,11-dihydro-5H-dibenz[b,e]azepine, 2.15 g of 4-nitrobenzoyl chloride, 1.50 g of N,N-diisopropylethylamine, 54 mg of 4-(dimethylamino)pyridine in 15 ml of dichloromethane is refluxed for 18 hours. The mixture is cooled and washed with H2O, 1N HCl, 1M NaHCO3, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrous magnesium silicate and the pad washed with dichloromethane. The filtrate is concentrated and the residue recrystallized from dichloromethane-hexane to give 2.33 g of crystals, m.p. 198°-201° C.

출처