反応 #581930

反応方程式

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

product 56

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

HCl

→

2-Amino-3-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-propionic acid-hydrochloride

溶媒

AcOH

water

反応条件

後処理

1. 1
   その他The precipitate formed
2. 2
   ろ過was filtered off
3. 3
   その他The filtrate was evaporated i
4. 4
   その他The precipitate formed
5. 5
   ろ過was filtered off
6. 6
   洗浄washed with EtOH
7. 7
   その他dried i
8. 8
   その他The crude product was used in the next reaction step without any further purification

実験手順

To a solution of 40.0 g (94.16 mmol) diethyl 2-acetylamino-2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-malonate (Intermediate product 56) in 110 mL AcOH and 150 mL water was added 50 mL conc. aqueous HCl and the reaction mixture was heated to 140° C. for 4 hours. The precipitate formed was filtered off and discarded. The filtrate was evaporated i. vac., combined with 100 mL EtOH and stirred for 15 minutes at RT. The precipitate formed was filtered off, washed with EtOH and dried i. vac. The crude product was used in the next reaction step without any further purification.

出典