HRID1634098
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 solution of 1-(4′-nitrophenyl)-5-bromo-3-methylpyrazole (138 mg, 0.49 mmol) in THF (5 mL) was added Pd(PPh3)4 (21 mg, 0.018 mmol) followed by vinyl tributyltin (0.16 mL, 0.54 mmol). The mixture was heated at reflux for 6 hr under N2, and was then quenched with saturated KF and extracted with EtOAc. The extract was dried over MgSO4 and concentrated. The residue was purified by column chromatography on silica gel (hexane/acetate, 10:1) to give the title compound (103 mg, 92%).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureat reflux for 6 hr under N2
- customwas then quenched with saturated KF
- extractionextracted with EtOAc
- dry with materialThe extract was dried over MgSO4
- concentrationconcentrated
- customThe residue was purified by column chromatography on silica gel (hexane/acetate, 10:1)