HRID280902

反应详情

EQUATION

反应方程式

HRID 280902 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 10-liter separable flask equipped with a stirrer, a condenser and a water separator, 2700 g of tricyclo [5.2.1.02,6 ]deca-8-ol (white crystal powder), 1896 g of methacrylic acid, 2700 g of toluence, 135 g of p-toluenesulfonic acid and 0.64 g of hydroquinone monomethyl ether were placed and reacted at 115° C. with stirring for 2 hours while removing the water generated out of the system. Then, the reaction solution was taken out of the flask and then subjected to distillation to remove low boiling point components. Then, 15 g of hydroquinone monomethyl ether was added to the resulting solution and distillation under reduced pressure was conducted to isolate a distillate having a boiling point of 90°-95° C. under 0.7 mmHg. The distillate was washed with an agueous solution of 2% KOH, washed with water, dehydrated and filtered to give tricyclo[5.2.1.02,6 ]deca-8-yl methacrylate (hereinafter referred to as "TCD-MA") in 80% yield and 99.5 % purity.

WORKUP

后处理

  1. customIn a 10-liter separable flask equipped with a stirrer, a condenser
  2. customreacted at 115° C.
  3. customwhile removing the water
  4. distillationsubjected to distillation
  5. customto remove low boiling point components
  6. additionThen, 15 g of hydroquinone monomethyl ether was added to the resulting solution and distillation under reduced pressure
  7. customto isolate a distillate
  8. washThe distillate was washed with an agueous solution of 2% KOH
  9. washwashed with water
  10. filtrationfiltered