HRID524382

反应详情

EQUATION

反应方程式

HRID 524382 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(4-Chlorosulfonyl-phenyl)-acetic acid methyl ester (13 g, 52.41 mmol) was taken in carbon tetrachloride (262 mL). N-Bromosuccinimide (10.26 g, 57.66 mmol) was added in one lot followed by benzoyl peroxide (1.39 g, 5.766 mmol). The reaction mixture was refluxed for 2 days. The reaction mixture was cooled to room temperature and filtered; filtrate was washed with water followed by brine solution, dried over anhydrous sodium sulfate and concentrated. Product was purified using column chromatography in 3% ethyl acetate:hexane which yielded bromo-(4-chlorosulfonyl-phenyl)-acetic acid methyl ester (2.8 g) as a gummy mass.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 2 days
  2. filtrationfiltered
  3. washfiltrate was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customProduct was purified