반응 #1552035

반응 방정식

tert-Octylamine

triethylamine

4-nitrobenzoyl chloride

→

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

수율 76.0%

용매

dichloroethane

반응 조건

후처리

1. 1
   온도The mixture is refluxed for 4 hours
2. 2
   workup.ADDITIONThe reaction mixture is poured into ice-cold water
3. 3
   추출the product is extracted with dichloromethane
4. 4
   기타drying
5. 5
   기타the solvent is evaporated off
6. 6
   기타The beige precipitate obtained
7. 7
   기타is recrystallized from a mixture of isopropyl ether and ethanol (10:1 ratio)

실험 절차

tert-Octylamine (51.7 g, 0.4 mol) and triethylamine (61.2 ml, 0.44 mol) in 260 ml of dichloroethane are introduced into 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 in 50 minutes. The mixture is refluxed for 4 hours. The reaction mixture is poured into ice-cold water; the product is extracted with dichloromethane, drying is carried out, and the solvent is evaporated off. The beige precipitate obtained is recrystallized from a mixture of isopropyl ether and ethanol (10:1 ratio). 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 it is in the following stage.

출처