HRID1680039

反应详情

EQUATION

反应方程式

HRID 1680039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

17.8 g (0.01 mol) of 3-formyl-benzoic acid ethyl ester, 13.6 g (0.1 mol) of phenylacetic acid and 10 g of triethylamine were dissolved in 30 ml of acetic anhydride and the solution was heated to the reflux for 5 hours. After cooling, 300 ml of water were added to the reaction mixture and the mixture was then heated to the boil for 20 minutes. The solid residue was then decanted off hot, and this was recrystallised from methanol, to which a little water had been added. 13 g (43.9% of theory) of 3-(2-carboxy-2-phenylvinyl)-benzoic acid ethyl ester were obtained as light yellow crystals of melting point 139°-140° C. (isomer mixture with a cis proportion of about 90%). ##STR60##

WORKUP

后处理

  1. temperaturethe solution was heated to the
  2. temperaturereflux for 5 hours
  3. temperatureAfter cooling
  4. temperaturethe mixture was then heated to the boil for 20 minutes
  5. customThe solid residue was then decanted off hot
  6. customthis was recrystallised from methanol, to which a little water
  7. additionhad been added