HRID1074420

反应详情

EQUATION

反应方程式

HRID 1074420 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-(4-ethoxyphenyl)propenoic acid ethyl ester (13.2 g) was mixed with benzene (7.5 ml), α-pinene (2 drops) N-ethyldiisopropyl amine (2 drops) and tetrafluoroethylene (15.5 ml) and heated to 150°-155° for 24 hours then 155°-60° C. for 17 hours. After evaporation of volatile materials the residue (16.6 g) was dissolved in dichloromethane and chromatographed on a column of silica gel to give the ester as a colourless oil 14.5 g (75%). Analysis: C 56.47%, H 5.24%, F 23.4%, C15H16F4O3 requires C 56.25%, H 5.04%, F. 23.7%.

WORKUP

后处理

  1. temperatureheated to 150°-155° for 24 hours
  2. customAfter evaporation of volatile materials the residue (16.6 g)
  3. dissolutionwas dissolved in dichloromethane
  4. customchromatographed on a column of silica gel