反応 #2275677

反応方程式

tert-Octylamine

triethyamine

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 heated
2. 2
   温度at reflux for 4 hours
3. 3
   workup.ADDITIONThe mixture is poured onto ice-cold water
4. 4
   抽出extraction
5. 5
   その他the extract is dried
6. 6
   その他the solvent is evaporated
7. 7
   その他The beige precipitate obtained
8. 8
   その他is recrystallized from a mixture of isopropyl ether and ethanol (ratio 10:1)

実験手順

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.

出典