HRID1037049

反应详情

EQUATION

反应方程式

HRID 1037049 的结构方程式

PROCEDURE

实验过程

To a solution of 3-bromo-4-(methoxycarbonyl)benzoic acid (3.0 g, 11.6 mmol) in MeOH (50 mL) was slowly added SOCl2 (2.76 g, 23.2 mmol) dropwise. After the addition completion, the reaction mixture was refluxed for 5 h. Then MeOH was removed and water was added. It was extracted with EA and the organic layer was washed with aqueous sodium bicarbonate solution, brine, dried over Na2SO4, filtered and concentrated under reduced pressure to give dimethyl 2-bromoterephthalate (3.1 g, yield 98%) as a white solid. It was used without further purification in the next step.

WORKUP

后处理

  1. temperatureAfter the addition completion, the reaction mixture was refluxed for 5 h
  2. customThen MeOH was removed
  3. additionwater was added
  4. extractionIt was extracted with EA
  5. washthe organic layer was washed with aqueous sodium bicarbonate solution, brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure