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
6,7-Dimethoxy-4-tri-n-butylstanniophenylmethyl)quinoline (82 mg) obtained in Example 162, commercially available 4-t-butylbenzoyl chloride (31 mg) and a catalytic amount of commercially available bis(triphenylphosphine)palladium(II) chloride were dissolved in chloroform (3 ml), and the admixture was stirred for 15 hours under reflux with heat. After the addition of water, the admixture was extracted with methylene chloride, and the organic layer was washed with brine and saturated aqueous potassium fluoride and then dried with anhydrous sodium sulfate. After removing the solvent by distillation, the resulting residue was purified by thin layer chromatography on silica gel eluting with hexane/ethyl acetate (2/1) to obtain 6 mg of the title compound (yield: 10%).
WORKUP
后处理
- temperatureunder reflux
- temperaturewith heat
- extractionthe admixture was extracted with methylene chloride
- washthe organic layer was washed with brine and saturated aqueous potassium fluoride
- dry with materialdried with anhydrous sodium sulfate
- customAfter removing the solvent
- distillationby distillation
- customthe resulting residue was purified by thin layer chromatography on silica gel eluting with hexane/ethyl acetate (2/1)