HRID917658

反应详情

EQUATION

反应方程式

HRID 917658 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

25 g (208 mmol) of o-tolualdehyde, 14.58 g (208 mmol) of methyl vinyl ketone, 21.05 g (208 mmol) of triethylamine, 5.4 g (21.4 mmol) of 3-ethyl-5-(2-hydroxyethyl)-4-methylthiazolium bromide were dissolved in this order in 100 ml of DMF and stirred at 80° C. for 12 hours. The reaction mixture was subsequently admixed with 400 ml of water and extracted twice with methylene chloride. The combined methylene chloride phases were washed with 10% strength sulfuric acid and saturated sodium hydrogencarbonate solution and dried over sodium sulfate. After taking off the solvent on a rotary evaporator, the product was purified by fractional distillation.

WORKUP

后处理

  1. extractionextracted twice with methylene chloride
  2. washThe combined methylene chloride phases were washed with 10% strength sulfuric acid and saturated sodium hydrogencarbonate solution
  3. dry with materialdried over sodium sulfate
  4. customon a rotary evaporator
  5. distillationthe product was purified by fractional distillation