HRID79016

反应详情

EQUATION

反应方程式

HRID 79016 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 4-(2-fluoro-4-trimethylsilanylphenylamino)-1-(toluene-4-sulfonyl)-1H-indazole-5-carboxylic acid methyl ester (0.56 g, 1.1 mmol) in DCM (3 mL) at 0° C. was added a solution of iodine monochloride in DCM (2.2 mL, 1M, 2.2 mmol). The reaction mixture was stirred at 0° C. for 30 minutes. The reaction was quenched by the addition of water (10 mL) then diluted with saturated aqueous sodium thiosulfate solution (10 mL). The resultant mixture was extracted with ethyl acetate (3×20 mL) and the combined organic fractions washed with brine (20 mL), dried (MgSO4) then concentrated in vacuo. The resultant residue was subjected to flash chromatography (SiO2, gradient 0-100% DCM in cyclohexane) to yield the title compound as a light brown solid (0.51 g, 83%). LCMS (Method B): RT=4.87 min, [M+H]+=566.

WORKUP

后处理

  1. customThe reaction was quenched by the addition of water (10 mL)
  2. additionthen diluted with saturated aqueous sodium thiosulfate solution (10 mL)
  3. extractionThe resultant mixture was extracted with ethyl acetate (3×20 mL)
  4. washthe combined organic fractions washed with brine (20 mL)
  5. dry with materialdried (MgSO4)
  6. concentrationthen concentrated in vacuo