HRID20593

反应详情

EQUATION

反应方程式

HRID 20593 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Trimethylsilyl iodide (0.080 mL, 0.559 mmol) was added to a solution of 3-[(1S)-2-methoxy-1-methylethoxy]-N-(1-methyl-1H-pyrazol-3-yl)-5-[4-(1H-pyrazol-3-yl)phenoxy]benzamide (50 mg, 0.112 mmol) in acetonitrile (2 mL) and the reaction mixture allowed to stir at RT for 18 hours. The reaction was diluted with ethyl acetate (15 mL) and quenched by the addition of saturated aqueous sodium bicarbonate solution (20 mL). The organic phase was washed with saturated aqueous thiosulphate solution (20 mL) and dried (MgSO4). The volatiles were removed under reduced pressure and the resulting oil purified by chromatography on silica, eluting with 0-100% ethyl acetate in iso-hexane, to give the title compound as a colourless solid (40 mg).

WORKUP

后处理

  1. customquenched by the addition of saturated aqueous sodium bicarbonate solution (20 mL)
  2. washThe organic phase was washed with saturated aqueous thiosulphate solution (20 mL)
  3. dry with materialdried (MgSO4)
  4. customThe volatiles were removed under reduced pressure
  5. customthe resulting oil purified by chromatography on silica
  6. washeluting with 0-100% ethyl acetate in iso-hexane