HRID907075

反应详情

EQUATION

反应方程式

HRID 907075 的结构方程式

PROCEDURE

实验过程

Acetyl chloride (12.5 ml, 175 mmol) was added to a suspension of 2,2′-(1,3-phenylene)diacetic acid (50.0 g, 260 mmol) in ethanol (500 ml) and the resulting solution heated to reflux for 16 hours. The reaction was cooled to room temperature and the solvent removed in vacuo. The residue was partitioned between saturated aqueous sodium hydrogencarbonate (300 ml) and ethyl acetate (500 ml). The organic phase was washed with water (200 ml), sat. aq. sodium chloride (300 ml), dried (sodium sulfate) and the solvent removed in vacuo to give the title compound as a pale yellow oil (63.5 g).

WORKUP

后处理

  1. temperaturethe resulting solution heated
  2. temperatureto reflux for 16 hours
  3. customthe solvent removed in vacuo
  4. customThe residue was partitioned between saturated aqueous sodium hydrogencarbonate (300 ml) and ethyl acetate (500 ml)
  5. washThe organic phase was washed with water (200 ml), sat. aq. sodium chloride (300 ml)
  6. dry with materialdried (sodium sulfate)
  7. customthe solvent removed in vacuo