HRID128470

反应详情

EQUATION

反应方程式

HRID 128470 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-[4-(2-Thienyl-hydroxyiminomethyl)-phenoxy]-2-methyl propionic acid (6.7 g) is dissolved in a sodium ethoxide solution in ethanol (100 ml; prepared from 1.3 g sodium), and the solution is then refluxed for 1 hour, after which dimethylformamide (75 ml) is added thereto and the ethanol is evaporated off. Butyl bromide (9 g) is added to the solution at 80° C. and the mixture is stirred for 3 hours, after which the solvent is evaporated under reduced pressure. Water and chloroform are then added to the resulting material. After stirring the mixture, the chloroform phase is decanted off and is then washed with an aqueous alkaline solution. After drying, the solvent is evaporated off and the desired ester is isolated as an oil consisting of an admixture of equivalent amounts of both stereoisomers Z/E. nd22 =1.545.

WORKUP

后处理

  1. temperaturethe solution is then refluxed for 1 hour
  2. customthe ethanol is evaporated off
  3. additionButyl bromide (9 g) is added to the solution at 80° C.
  4. customafter which the solvent is evaporated under reduced pressure
  5. additionWater and chloroform are then added to the resulting material
  6. stirringAfter stirring the mixture
  7. customthe chloroform phase is decanted off
  8. washis then washed with an aqueous alkaline solution
  9. customAfter drying
  10. customthe solvent is evaporated off