HRID2283295

反应详情

EQUATION

反应方程式

HRID 2283295 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 2-(3-bromobenzenesulfonylamino)-5-methyl-benzensulfonamide (1.50 g, 3.70 mmol), 3,4-dichlorobenzeneboronic acid (0.84 g, 4.44 mmol), tricyclohexyl phosphine (0.45 g, 1.60 mmol) and potassium phosphate (3 g, 14.15 mmol) in DMF (10 mL), was added Pd(OAc)2 (0.17 g, 0.74 mmol). The reaction mixture was stirred at 80° C. for 10 h, 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 (0.9 g, 51%).

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