HRID1977003

反应详情

EQUATION

反应方程式

HRID 1977003 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
37 °C

PROCEDURE

实验过程

Methacrylic anhydride (6.92 g; 0.045 moles) was added dropwise to a chilled solution of purified 4-allyloxyphenol (7.0 g; 0.047 moles), triethylamine (3.55 g; 0.035 moles), 4-dimethylaminopyridine (0.43 g; 0.004 moles), 2-6-di-tert-butyl-4-methylphenol (0.018 g; 0.08 m moles) and toluene (20 ml) in a stirred 100 ml reaction flask fitted with a reflux condenser, magnetic stirrer and thermocouple probe. During the addition the reaction temperature increased to 37° C. The mixture was heated at 110° C. for 1.5 hour, cooled and washed sequentially with equal volumes of saturated sodium bicarbonate, dilute hydrochloric acid and water. The solution was dried over magnesium sulfate and the solvent removed under reduced pressure to yield 4-allyloxyphenyl methacrylate (8.3 g; 90% yield) as a clear yellow liquid. The structure of the monomer was confirmed by proton and infrared spectral analysis and GC analysis indicated a purity of 90%.

WORKUP

后处理

  1. customfitted with a reflux condenser, magnetic stirrer
  2. additionDuring the addition the reaction temperature
  3. temperatureThe mixture was heated at 110° C. for 1.5 hour
  4. temperaturecooled
  5. washwashed sequentially with equal volumes of saturated sodium bicarbonate, dilute hydrochloric acid and water
  6. dry with materialThe solution was dried over magnesium sulfate
  7. customthe solvent removed under reduced pressure