反応 #581929

反応方程式

2-chloro-4-chlormethyl-6-trifluoromethyl-phenylamine

product 55

2-chloro-4-chlormethyl-6-trifluoromethyl-phenylamine

diethyl 2-acetylamino-malonate

sodium

EtOH

→

Diethyl 2-acetylamino-2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-malonate

溶媒

1,4-dioxane

water

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture was stirred for a further 16 hours
2. 2
   その他The precipitate formed
3. 3
   ろ過was filtered off
4. 4
   洗浄washed with water
5. 5
   その他dried i

実験手順

24.11 g (0.11 mol) diethyl 2-acetylamino-malonate was added to a freshly prepared solution of 2.55 g (0.11 mol) sodium in 200 mL abs. EtOH under a nitrogen atmosphere and the mixture was stirred for 15 minutes at RT. A solution of 27.00 g (0.11 mol) 2-chloro-4-chlormethyl-6-trifluoromethyl-phenylamine (Intermediate product 55) in 100 mL 1,4-dioxane was rapidly added dropwise and the mixture was stirred for 4 hours at RT. 500 mL water were added and the mixture was stirred for a further 16 hours. The precipitate formed was filtered off, washed with water and dried i. vac.

出典