HRID902621
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
A mixture of (3-iodo-phenyl)-acetic acid methyl ester (948 mg, 3.4 mmol), 1-(t-butyldimethylsilyloxy)but-3-yne (644 mg, 3.5 mmol), copper(1)iodide (50 mg), and bis(triphenylphosphine)-palladium(II)chloride (50 mg) in Et3N (5 ml) was refluxed, under argon for 2 hr. The reaction was cooled, and the liquid was decanted off, diluted with diethyl ether, and washed with 1N HCl. The organic layer was dried and the solvent was evaporated. The residue was chromatographed on silica gel (hexane/methylene chloride 60/40) to give the title compound as an oil (700 mg, 62%). MS (ESI) 333.0 (M+H)+.
WORKUP
后处理
- temperaturewas refluxed, under argon for 2 hr
- temperatureThe reaction was cooled
- customthe liquid was decanted off
- additiondiluted with diethyl ether
- washwashed with 1N HCl
- customThe organic layer was dried
- customthe solvent was evaporated
- customThe residue was chromatographed on silica gel (hexane/methylene chloride 60/40)