反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- extractionthe product was extracted with ethyl acetate
- customThe organic phase was separated
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo
- customThe crude product was purified by flash column chromatography