HRID1492955
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter heating
- temperatureto reflux for 2 hrs
- distillationthe solvent is distilled off
- additionwater is added
- temperaturethe mixture refluxed for a further hour
- extractionExtraction
- customwith methylene chloride and evaporation