반응 #7632

반응 방정식

ethyl chloro(oxo)acetate

2-(acetylamino)butanoic acid

pyridine

→

Ethyl 3-(acetylamino)-2-oxopentanoate

용매

tetrahydro-furane

반응 조건

후처리

1. 1
   온도heated
2. 2
   온도While heating
3. 3
   온도at reflux
4. 4
   온도The reaction mixture is heated
5. 5
   온도at reflux until no more evolution of gas
6. 6
   추출the organic phase extracted with ethyl acetate
7. 7
   기타The dried organic phase is evaporated to dryness in vacuo
8. 8
   workup.DISSOLUTIONdissolved in ethanol
9. 9
   기타the solution directly used for the next reaction

실험 절차

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.

출처