HRID1460852

反应详情

EQUATION

反应方程式

HRID 1460852 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In the same reactor as used in Example 1, 760 kg (5 kmoles) of tricyclo[5.2.1.02,6 ]deca-8-yl alcohol and 1500 kg (15 kmole) of methyl methacrylate were placed and well mixed with stirring. The water content of the resulting mixture was 2500 ppm. To the mixture, 550 g of hydroquinone monomethyl ether was added and heated while introducing thereinto dried air at a rate of 4 m3/ hr and reluxing methyl methacrylate through the distillation column to remove water by azeotropic distillation. After 1 hour from the beginning of the reflux of methyl methacrylate, the water content in the reactor became 630 ppm. Then, 3 kg of anhydrous lithium hydroxide was charged into the reactor to carry out the reaction. While removing methanol by-produced by the reaction from the reaction system by distillation, the reaction was continued until almost no methanol was distilled (about 7 hours), followed by removal of unreacted methyl methacrylate under reduced pressure. After cooling, the mixture was filtered under pressure (2 kg/cm2) using a filter paper (pore size 0.1 mm, area 5 m2) placing thereon 10 kg of diatomaceous earth to yield 990 kg of tricyclo[5.2.1.02,6 ]deca-8-yl methacrylate with the filtrating time of 2 hours.

WORKUP

后处理

  1. additionwell mixed
  2. temperatureheated
  3. additionwhile introducing
  4. dry with materialthereinto dried air at a rate of 4 m3/ hr and reluxing methyl methacrylate
  5. distillationthrough the distillation column
  6. customto remove water
  7. distillationby azeotropic distillation
  8. temperatureAfter 1 hour from the beginning of the reflux of methyl methacrylate
  9. additionThen, 3 kg of anhydrous lithium hydroxide was charged into the reactor
  10. customthe reaction
  11. customWhile removing methanol
  12. customby-produced by the reaction from the reaction system by distillation
  13. distillationwas distilled (about 7 hours)
  14. customfollowed by removal of unreacted methyl methacrylate under reduced pressure
  15. temperatureAfter cooling
  16. filtrationthe mixture was filtered under pressure (2 kg/cm2)