HRID628554

反应详情

EQUATION

反应方程式

HRID 628554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

92.12 g (0.5 mol) of 1,3,5-adamantanetriol are suspended in 153.14 g (1.5 mol) of acetic anhydride. Subsequently, 10 drops of concentrated sulfuric acid are added and the mixture is stirred on a rotary evaporator (without vacuum) until a homogeneous solution has formed. Subsequently, the mixture is heated to 100° C. under reflux for 2 h. After cooling, the reaction mixture is added to 300 ml of ice-water and extracted with dichloromethane. The combined organic phases are deacidified with sodium carbonate solution and washed with water. The mixture is dried over magnesium sulfate and filtered, and the solvent is removed under reduced pressure. 150.50 g (0.48 mol; 97.0%) of a colorless oil are obtained.

WORKUP

后处理

  1. customhas formed
  2. temperatureunder reflux for 2 h
  3. temperatureAfter cooling
  4. extractionextracted with dichloromethane
  5. washwashed with water
  6. dry with materialThe mixture is dried over magnesium sulfate
  7. filtrationfiltered
  8. customthe solvent is removed under reduced pressure
  9. custom150.50 g (0.48 mol; 97.0%) of a colorless oil are obtained