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 mixture of 4-chlorobiphenyl (23 mg, 0.12 mmol), 1,4-dioxane (2 ml) and water (200 μl) were added potassium acetoxymethyl trifluoroborate (44 mg, 0.24 mmol), palladium (II) acetate (14 mg, 0.061 mmol), 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (50 mg, 0.12 mmol), and potassium phosphate (170 mg, 0.73 mmol) at room temperature. The reaction mixture was heated to reflux overnight under the nitrogen atmosphere. After the reaction mixture was cooled at room temperature, water and ethyl acetate were added to the mixture. After the organic layer was washed with an aqueous saturated sodium chloride solution, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (heptane:ethyl acetate=2:1) to obtain the title compound (18 mg, 0.098 mmol, 80%).
WORKUP
后处理
- temperatureThe reaction mixture was heated
- temperatureto reflux overnight under the nitrogen atmosphere
- washAfter the organic layer was washed with an aqueous saturated sodium chloride solution
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was purified by silica gel column chromatography (heptane:ethyl acetate=2:1)