반응 #2275677

반응 방정식

tert-Octylamine

triethyamine

4-nitrobenzoyl chloride

→

4-nitro-N-(tert-octyl)benzamide

수율 76.0%

용매

dichloroethane

반응 조건

후처리

1. 1
   온도The mixture is heated
2. 2
   온도at reflux for 4 hours
3. 3
   workup.ADDITIONThe mixture is poured onto ice-cold water
4. 4
   추출extraction
5. 5
   기타the extract is dried
6. 6
   기타the solvent is evaporated
7. 7
   기타The beige precipitate obtained
8. 8
   기타is recrystallized from a mixture of isopropyl ether and ethanol (ratio 10:1)

실험 절차

tert-Octylamine (51.7 g, 0.4 mol) and triethyamine (61.2 ml, 0.44 mol) are introduced into 260 ml of dichloroethane in a reactor. The mixture is heated to 70° C. and then 4-nitrobenzoyl chloride (77.9 g, 0.42 mol) is added in small portions over 50 minutes. The mixture is heated at reflux for 4 hours. The mixture is poured onto ice-cold water; extraction is carried out with dichloromethane, the extract is dried and the solvent is evaporated. The beige precipitate obtained is recrystallized from a mixture of isopropyl ether and ethanol (ratio 10:1). After drying under vacuum, 84.6 g (Yield 76%) of 4-nitro-N-(tert-octyl)benzamide are obtained in the form of an off-white powder which is used as is in the following stage.

출처