反応 #7632

反応方程式

ethyl chloro(oxo)acetate

2-(acetylamino)butanoic acid

pyridine

→

Ethyl 3-(acetylamino)-2-oxopentanoate

溶媒

tetrahydro-furane

反応条件

後処理

1. 1
   温度heated
2. 2
   温度While heating
3. 3
   温度at reflux
4. 4
   温度The reaction mixture is heated
5. 5
   温度at reflux until no more evolution of gas
6. 6
   抽出the organic phase extracted with ethyl acetate
7. 7
   その他The dried organic phase is evaporated to dryness in vacuo
8. 8
   workup.DISSOLUTIONdissolved in ethanol
9. 9
   その他the solution directly used for the next reaction

実験手順

9.2 g (63.4 mmol) 2-(acetylamino)butanoic acid are suspended in 120 ml tetrahydro-furane and heated to reflux together with 15.0 g (190 mmol) pyridine and a bit of N,N-dimethylaminopyridine. While heating at reflux, 17.3 g (127 mmol) ethyl chloro(oxo)acetate are added dropwise. The reaction mixture is heated at reflux until no more evolution of gas can be observed. After cooling down to room temperature, the reaction mixture is added to ice water and the organic phase extracted with ethyl acetate. The dried organic phase is evaporated to dryness in vacuo, dissolved in ethanol and the solution directly used for the next reaction.

出典