反応 #2275679

反応方程式

tert-butylamine

triethylamine

4-Nitrobenzoyl chloride

→

N-(tert-butyl)-4-nitrobenzamide

収率 77.0%

溶媒

dichloromethane

methylene chloride

反応条件

後処理

1. 1
   workup.WAITleft
2. 2
   洗浄The organic phase is washed twice with water
3. 3
   その他dried
4. 4
   その他After removing the solvent under reduced pressure
5. 5
   その他the solid obtained
6. 6
   その他is recrystallized from isopropanol

実験手順

4-Nitrobenzoyl chloride (18.9 g, 0.1 mol) dissolved in 60 ml of methylene chloride is added, over 30 minutes at a temperature of 0-5° C., to a solution of tert-butylamine (8.3 g, 0.112 mol) and of triethylamine (15.6 ml, 0.112 mol) dissolved in 170 ml of dichloromethane in a reactor. The reaction mixture is brought back to laboratory temperature and left stirring for 2 hours. The organic phase is washed twice with water and dried. After removing the solvent under reduced pressure, the solid obtained is recrystallized from isopropanol. 17.1 g (Yield: 77%) of N-(tert-butyl)-4-nitrobenzamide are obtained in the form of a pale yellow powder (m.p. 161-2° C.) which is used as is in the following stage.

出典