HRID2081312

反应详情

EQUATION

反应方程式

HRID 2081312 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

1.34 g of (4-(2-iodophenoxy)-butyric acid ethyl ester and 6.4 g of (E)-1,2-bis-(tri-n-butylstannyl)-ethylene (50%) are dissolved in 12 ml of toluene, mixed with 94 mg of tetrakis-(triphenylphosphine)-palladium and heated with stirring and argon atmosphere for 2 hours to 70°-80° C. (bath temperature). After cooling to room temperature, the reaction mixture is diluted with 12 ml of diethyl ether and treated with a solution of 2.04 g of iodine in 10 ml of diethyl ether, worked up and chromatographed on silica gel with n-hexane/ethyl acetate=95/5 under the conditions of example 2C. 900 mg of 4-[-[(E)-2-iodovinyl]-phenoxy]-butyric acid ethyl ester is obtained as a yellow oil.

WORKUP

后处理

  1. temperatureheated
  2. customchromatographed on silica gel with n-hexane/ethyl acetate=95/5 under the conditions of example 2C