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
To a suspension of 308 mg (1.62 mmol, 25 mol %) of copper (I) iodide in 30 mL of THF was added dropwise vinylmagnesium bromide as a 1 M solution in THF at −50° C. After stirring for 10 min, a solution of 1.5 g (6.49 mmol) of 3,5-dimethoxybenzyl bromide in 8 mL of THF was added, and the resulting solution was stirred at −30° C. for 1 h and then was warmed to room temperature. The reaction mixture was quenched by the slow addition of 20 mL of water. After stirring for 5 min, the layers were separated and the aqueous layer was extracted twice with 20-mL portions of ethyl acetate. The combined organic fractions were dried (Na2SO4), filtered through a plug of silica gel (eluted with ethyl acetate) and concentrated in vacuo to afford 1.2 g (100%) of product as a yellow oil.
WORKUP
后处理
- stirringthe resulting solution was stirred at −30° C. for 1 h
- customThe reaction mixture was quenched by the slow addition of 20 mL of water
- stirringAfter stirring for 5 min
- customthe layers were separated
- extractionthe aqueous layer was extracted twice with 20-mL portions of ethyl acetate
- dry with materialThe combined organic fractions were dried (Na2SO4)
- filtrationfiltered through a plug of silica gel (eluted with ethyl acetate)
- concentrationconcentrated in vacuo