HRID128615

反应详情

EQUATION

反应方程式

HRID 128615 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of ethyl formate (55.2 g) and ethyl propionate (51.0 g) was added dropwise with stirring to a suspension of sodium hydride (20.9 g, 60% dispersion in mineral oil) in dry THF (260 ml) under nitrogen. On completion of the addition, the temperature of the reaction mixture rose gradually from ambient temperature to 45° C. accompanied by rapid evolution of hydrogen. The reaction mixture was stirred for 2 hours then cooled and water (400 ml) was added cautiously. The basic solution was washed with ether, then acidified with dilute hydrochloric acid and extracted with ether to give an oil. The oil was distilled and the fraction boiling in the range 100°-160° C. was collected to give ethyl 2-formylpropionate.

WORKUP

后处理

  1. additionwas added dropwise
  2. additionOn completion of the addition
  3. customrose gradually from ambient temperature to 45° C.
  4. temperaturethen cooled
  5. washThe basic solution was washed with ether
  6. extractionextracted with ether
  7. customto give an oil
  8. distillationThe oil was distilled
  9. customboiling in the range 100°-160° C.
  10. customwas collected