HRID992994

反应详情

EQUATION

反应方程式

HRID 992994 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

THF (5 mL) was added to sodium hydride (55% dispersion in mineral oil, 162 mg) under an argon atmosphere, and a solution of ethyl diethylphosphonoacetate (832 mg) in THF (2 mL) was added dropwise to the mixture at −10° C. After 30 minutes, a solution of 2-(3,4,5-trimethoxyphenyl)thiazole-4-carboaldehyde (942 mg) in THF (8 mL) was slowly added to the resultant mixture, and the mixture was warmed to room temperature over 30 minutes and then stirred for 2 hours. The reaction mixture was diluted with ethyl acetate, washed with a saturated aqueous solution of sodium hydrogencarbonate, water and saturated brine, dried over anhydrous sodium sulfate. After concentrating the reaction mixture under reduced pressure, the resultant crude crystals were recrystallized from ethyl acetate-hexane to obtain the title compound.

WORKUP

后处理

  1. washwashed with a saturated aqueous solution of sodium hydrogencarbonate, water and saturated brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationAfter concentrating the reaction mixture under reduced pressure
  4. customthe resultant crude crystals were recrystallized from ethyl acetate-hexane