HRID1637301

反应详情

EQUATION

反应方程式

HRID 1637301 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

118.4 g (0.29 mol) of this ester were dissolved in 50 ml of dimethylformamide at 70° C., 0.3 g of 2-tert-butyl-4,6-dimethylphenol was added as stabilizer, 111.7 g (0.9 mol) of dry potassium methacrylate salt were added, and the mixture was diluted with 70 ml of toluene. The reaction mixture was stirred at 100° C. for 6 h, then cooled and diluted with 800 ml of methyl tert-butyl ether. The precipitate was filtered off with suction, and the washing solution and the filtrate were combined and washed three times with water. They were then concentrated, and the crude product obtained was recrystallized from isopropanol. 4-(4-Methacryloyloxybutoxy)phenyl 4-allyloxybenzoate of m.p. 62-63° C. was obtained in a yield of 83%. Between 41 and 45° C. the ester has a nematic phase which occurs only on supercooling.

WORKUP

后处理

  1. additionwere added
  2. temperaturecooled
  3. filtrationThe precipitate was filtered off with suction
  4. washwashed three times with water
  5. concentrationThey were then concentrated
  6. customthe crude product obtained
  7. customwas recrystallized from isopropanol