反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwell mixed
- temperatureheated
- additionwhile introducing
- dry with materialthereinto dried air at a rate of 4 m3/ hr and reluxing methyl methacrylate
- distillationthrough the distillation column
- customto remove water
- distillationby azeotropic distillation
- temperatureAfter 1 hour from the beginning of the reflux of methyl methacrylate
- additionThen, 3 kg of anhydrous lithium hydroxide was charged into the reactor
- customthe reaction
- customWhile removing methanol
- customby-produced by the reaction from the reaction system by distillation
- distillationwas distilled (about 7 hours)
- customfollowed by removal of unreacted methyl methacrylate under reduced pressure
- temperatureAfter cooling
- filtrationthe mixture was filtered under pressure (2 kg/cm2)