HRID1064555

反应详情

EQUATION

反应方程式

HRID 1064555 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
30 °C

PROCEDURE

实验过程

19 g (0.1 mol) of methyl 3-(4,4,4-trifluoro-3-oxo-1-butenylamino)acrylate were dissolved in 200 ml of methanol in a three-neck flask and 1 g of Li2CO3 was added. The reaction mixture was heated for 6-8 h under reflux, cooled to 30° C. and 10 ml of aqueous HCl were added. The reaction mixture was stirred for 1 h, the methanol removed under reduced pressure and the product extracted with diethyl ether. The solvent was removed and methyl 4-trifluoronicotinate purified by vacuum distillation. 14 g (81%) of the product having a boiling point of 80° C./18 mbar were obtained.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated for 6-8 h
  2. temperatureunder reflux
  3. customthe methanol removed under reduced pressure
  4. extractionthe product extracted with diethyl ether
  5. customThe solvent was removed
  6. distillationmethyl 4-trifluoronicotinate purified by vacuum distillation
  7. customwere obtained