HRID598072

反应详情

EQUATION

反应方程式

HRID 598072 的结构方程式

PROCEDURE

实验过程

A mixture of 5-methoxy-3-methyl-1H-quinazoline-2,4-dione (165 mg, 0.800 mmol) and N,N-diisopropylethylamine (0.307 ml, 1.76 mmol) in phosphorus oxychloride (2.2 ml, 24.0 mmol) was refluxed for 18 h with stirring and concentrated to dryness under vacuum. The residue was diluted with water. The aqueous solution was extracted with dichloromethane. The extract was washed with water, dried over magnesium sulfate and concentrated under vacuum to afford 179 mg (99%) of the title compound. The residue was used for the next reaction without further purification.

WORKUP

后处理

  1. temperaturewas refluxed for 18 h
  2. concentrationconcentrated to dryness under vacuum
  3. additionThe residue was diluted with water
  4. extractionThe aqueous solution was extracted with dichloromethane
  5. washThe extract was washed with water
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under vacuum