HRID1654722

反应详情

EQUATION

反应方程式

HRID 1654722 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-bromo-5-hydroxymethyltoluene (87.4 g) in methylene chloride (350 ml) were added, under ice-cooling with stirring, trietylamine (72.7 ml) and 4-dimethylaminopyridine (DMAP)(500 mg), and then thereto was added t-butyldimethylsilyl chloride (65.5 g). The mixture was stirred at 0° C. for 15 minutes, and stirred at room temperature for 3 hours. The reaction mixture is filtrated, and the filtrate was concentrated under reduced pressure. To the residure was added water (100 ml), and the mixture was extracted with ethyl acetate.

WORKUP

后处理

  1. temperaturecooling
  2. stirringThe mixture was stirred at 0° C. for 15 minutes
  3. stirringstirred at room temperature for 3 hours
  4. filtrationThe reaction mixture is filtrated
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. additionTo the residure was added water (100 ml)
  7. extractionthe mixture was extracted with ethyl acetate