反应 #7645

ord-806f557d0a9c4151b5de0201eb12a922

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  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
    萃取the organic phase extracted with ethyl acetate
  7. 7
    其他The dried organic phase is evaporated to dryness in vacuo
  8. 8
    workup.DISSOLUTIONdissolved in ethanol
  9. 9
    其他the solution directly used for the next reaction

实验过程

1.6 g (8 mmol) 2-[(cyclopentylcarbonyl)amino]butanoic acid are suspended in 30 ml tetrahydrofurane and heated to reflux together with 1.91 g (24 mmol) pyridine and a bit of N,N-dimethylaminopyridine. While heating at reflux, 2.19 g (16 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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07087605B2uspto-grants-2006_08