HRID1761269

反应详情

EQUATION

反应方程式

HRID 1761269 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A flask is charged with 66.5 g of acetic anhydride, 66.5 g of ammonium acetate, and 100 g of 1,1-cyclohexane diacetic acid. The reaction mass is heated to 160° C.-170° C. for eight hours, eliminating by distillation the acetic acid that has formed. It is cooled to 90° C.-110° C., and 200 g of water and 100 g of secondary butyl alcohol are added. It then undergoes further cooling to room temperature, and the pH is brought to approximately 9 using 30% of aqueous ammonia. This is followed by filtration, washing the solid with water. 87.7 g of dry 3,3-pentamethylene glutarimide are obtained (yield 97%).

WORKUP

后处理

  1. temperatureThe reaction mass is heated to 160° C.-170° C. for eight hours
  2. distillationeliminating by distillation the acetic acid that
  3. customhas formed
  4. temperatureIt is cooled to 90° C.-110° C.
  5. filtrationThis is followed by filtration
  6. washwashing the solid with water