HRID1973870

反应详情

EQUATION

反应方程式

HRID 1973870 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 20.8 g of 2-phenylquinazolin-4(3H)-one and 195 ml of thionyl chloride was slowly added 6.85 g of dimethylformamide and the mixture was heated under reflux for 75 minutes. The mixture was poured into 1000 ml of ice and the ice allowed to melt. The precipitate was collected by filtration to give a tan solid, m.p. 135°. The still-moist solid was dissolved in methylene chloride, the solution was dried over magnesium sulfate and was filtered. The filtrate was evaporated to dryness and the residue recrystallized from hexane to give 10.45 g of 4-chloro-2-phenylquinazoline which melted at 127°-128.5°.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 75 minutes
  3. filtrationThe precipitate was collected by filtration
  4. customto give a tan solid, m.p. 135°
  5. dry with materialthe solution was dried over magnesium sulfate
  6. filtrationwas filtered
  7. customThe filtrate was evaporated to dryness
  8. customthe residue recrystallized from hexane