تفاعل #7632

معادلة التفاعل

ethyl chloro(oxo)acetate

2-(acetylamino)butanoic acid

pyridine

→

Ethyl 3-(acetylamino)-2-oxopentanoate

المذيبات

tetrahydro-furane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheated
2. 2
   درجة الحرارةWhile heating
3. 3
   درجة الحرارةat reflux
4. 4
   درجة الحرارةThe reaction mixture is heated
5. 5
   درجة الحرارةat reflux until no more evolution of gas
6. 6
   استخلاصthe organic phase extracted with ethyl acetate
7. 7
   أخرىThe dried organic phase is evaporated to dryness in vacuo
8. 8
   workup.DISSOLUTIONdissolved in ethanol
9. 9
   أخرىthe solution directly used for the next reaction

الإجراء التجريبي

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.

المصدر