HRID2081312
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheated
- customchromatographed on silica gel with n-hexane/ethyl acetate=95/5 under the conditions of example 2C