HRID2079604

反应详情

EQUATION

反应方程式

HRID 2079604 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a solution of N-(4-chlorophenyl)-3-methoxy-benzenesulfonamide (900 mg, 3.02 mmol) in anhydrous THF (40 mL) was added sodium hydride (146 mg, 3.62 mmol) at 0-5° C. under nitrogen. The mixture was stirred at 25° C. for 30 minutes. Methyl bromoacetate (463 mg, 3.02 mmol) was then added, stirred for 1 h at 25° C. A further amount of methyl bromoacetate (232 mg, 1.51 mmol) was added, and stirring continued for another 12 h. The reaction mixture was quenched with saturated aqueous ammonium chloride solution, and extracted with ethyl acetate (3×20 ml). The combined organic layer was washed with water, dried (Na2SO4), evaporated under reduced pressure to yield the title compound as oily compound, which was used as such in the next step. Yield: 1.03 g (92%).

WORKUP

后处理

  1. stirringstirred for 1 h at 25° C
  2. stirringstirring
  3. waitcontinued for another 12 h
  4. customThe reaction mixture was quenched with saturated aqueous ammonium chloride solution
  5. extractionextracted with ethyl acetate (3×20 ml)
  6. washThe combined organic layer was washed with water
  7. dry with materialdried (Na2SO4)
  8. customevaporated under reduced pressure