HRID1492955

反应详情

EQUATION

反应方程式

HRID 1492955 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a nitrogen atmosphere, to 300 g powdered potassium carbonate in 1.5 1 of acetone is added 121 g II under stirring, followed by 83 ml of dimethyl sulphate. After heating to reflux for 2 hrs, the solvent is distilled off, water is added and the mixture refluxed for a further hour. Extraction with methylene chloride and evaporation gives 125 g of crude III, which is purified by crystallization from EtOAc, m.p. 118°-120°.

WORKUP

后处理

  1. temperatureAfter heating
  2. temperatureto reflux for 2 hrs
  3. distillationthe solvent is distilled off
  4. additionwater is added
  5. temperaturethe mixture refluxed for a further hour
  6. extractionExtraction
  7. customwith methylene chloride and evaporation