反応 #1552035

反応方程式

tert-Octylamine

triethylamine

4-nitrobenzoyl chloride

→

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

収率 76.0%

溶媒

dichloroethane

反応条件

後処理

1. 1
   温度The mixture is refluxed for 4 hours
2. 2
   workup.ADDITIONThe reaction mixture is poured into ice-cold water
3. 3
   抽出the product is extracted with dichloromethane
4. 4
   その他drying
5. 5
   その他the solvent is evaporated off
6. 6
   その他The beige precipitate obtained
7. 7
   その他is recrystallized from a mixture of isopropyl ether and ethanol (10:1 ratio)

実験手順

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.

出典