反応 #538519

反応方程式

2,2-difluoroethylamine

ethyl 4-chloroacetoacetate

acetic acid

toluene

→

ethyl 4-chloro-3-(2,2-difluoroethylamino)but-2-enecarboxylate

収率 98.0%

溶媒

ethanol

反応条件

後処理

1. 1
   温度At 10° C.-30° C., with cooling
2. 2
   workup.ADDITIONare added dropwise
3. 3
   その他the solvent is removed under reduced pressure at temperatures of down to 35° C

実験手順

To a solution of 197.2 g of ethyl 4-chloroacetoacetate in 1080 ml of toluene are added 13.3 ml of acetic acid. At 10° C.-30° C., with cooling, 100 g of 2,2-difluoroethylamine dissolved in 360 ml of ethanol are added dropwise. Subsequently, the mixture is stirred at room temperature for 8 h and the solvent is removed under reduced pressure at temperatures of down to 35° C. 278 g of ethyl 4-chloro-3-(2,2-difluoroethylamino)but-2-enecarboxylate are obtained in a purity of 93% (this corresponds to 98% yield).

出典