HRID522129

反应详情

EQUATION

反应方程式

HRID 522129 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-bromo-2-chloro-N-(3-cyano-1-phenyl-1H-pyrazol-5-yl)benzamide (Preparation 15, 500 mg, 1.24 mmol) in DMSO (5 mL) was added K2CO3 (340 mg, 2.48 mmol) followed by H2O2 (50% by weight, aqueous solution, 1.69 mL, 24.9 mmol). The reaction was stirred at room temperature for 3 hours. The reaction was quenched by the addition of saturated aqueous KHSO4 solution (5 mL) followed by water (15 mL) and EtOAc (40 mL). The mixture was filtered and separated. The organic layer was washed with brine (40 mL), dried over MgSO4, and concentrated in vacuo. The residue was slurried in water and filtered to afford the title compound (457 mg, 88%).

WORKUP

后处理

  1. customThe reaction was quenched by the addition of saturated aqueous KHSO4 solution (5 mL)
  2. filtrationThe mixture was filtered
  3. customseparated
  4. washThe organic layer was washed with brine (40 mL)
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo
  7. filtrationfiltered