HRID602045

反应详情

EQUATION

反应方程式

HRID 602045 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of AD-mix-α (50.0 g), t-BuOH (250 mL), and H2O (280 mL) was stirred until no solid was observed and then cooled to 0° C. Ethyl 3-(3-ethenyl-4,5-difluorophenyl)pentanoate (12.58 g, 0.0469 mol) in t-BuOH (35 mL) and H2O (10 mL) was added and the reaction stirred at 0° C. for 6 h and then warmed to room temperature overnight. Sodium sulfite (64 g) was added to quench the reaction and the reaction was diluted with H2O and extracted three times with ethylacetate. The combined organic layers were dried over Na2SO4, filtered, and concentrated. Column chromatography (hexane:ethylacetate, 7:3) yielded the desired product (13.02 g, 92%).

WORKUP

后处理

  1. temperaturewarmed to room temperature overnight
  2. customto quench
  3. customthe reaction
  4. extractionextracted three times with ethylacetate
  5. dry with materialThe combined organic layers were dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated