HRID2283298

反应详情

EQUATION

反应方程式

HRID 2283298 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

Pd(OAc)2 (44 mg, 0.19 mmol) was added to a solution of 2-(3-bromobenzenesulfonylamino)-5-methyl-benzensulfonamide (Example 150a) (0.40 g, 0.98 mmol), 3-(trifluoromethoxy)benzeneboronic acid (0.61 g, 2.96 mmol), tricyclohexyl phosphine (82 mg, 0.29 mmol) and potassium phosphate (0.42 g, 1.19 mmol) in toluene (10 mL). A few drops of water were added and the reaction mixture was stirred at 110° C. overnight. The reaction mixture was then diluted with 1N HCl and the product was extracted with ethyl acetate. The organic phase was separated, dried over sodium sulfate and concentrated in vacuo. The crude product was purified by flash column chromatography using ethyl acetate/hexane (1:3) to afford the title compound (140 mg, 30%).

WORKUP

后处理

  1. extractionthe product was extracted with ethyl acetate
  2. customThe organic phase was separated
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe crude product was purified by flash column chromatography