HRID2165007

反应详情

EQUATION

反应方程式

HRID 2165007 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1,1-Bis(2-hydroxyphenyl)ethanol (8.57 g) dissolved in 40 ml of dichloromethane was cooled with an ice bath and to this was added sequentially with stirring 3.70 ml of trifluoroacetic acid in 20 ml of dichloromethane and (dropwise) 7.67 ml of triethylsilane in 20 ml of dichloromethane. The mixture was allowed to warm to room temperature and react for another 2 hours. Ether and water were added and the phases separated. The organic phase was extracted with several small portions of 2N sodium hydroxide and the extracts were combined and acidified with hydrochloric acid. The resulting mixture was extracted with ether and the ether extract was dried over magnesium sulfate, filtered, and concentrated by evaporation under reduced pressure to obtain 6.10 g of the title compound as a brown oil.

WORKUP

后处理

  1. temperaturewas cooled with an ice bath
  2. additionto this was added sequentially
  3. customreact for another 2 hours
  4. customthe phases separated
  5. extractionThe organic phase was extracted with several small portions of 2N sodium hydroxide
  6. extractionThe resulting mixture was extracted with ether
  7. extractionthe ether extract
  8. dry with materialwas dried over magnesium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated by evaporation under reduced pressure