HRID1634098

反应详情

EQUATION

反应方程式

HRID 1634098 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 6 hr under N2
  3. customwas then quenched with saturated KF
  4. extractionextracted with EtOAc
  5. dry with materialThe extract was dried over MgSO4
  6. concentrationconcentrated
  7. customThe residue was purified by column chromatography on silica gel (hexane/acetate, 10:1)