HRID398027

反应详情

EQUATION

反应方程式

HRID 398027 的结构方程式

PROCEDURE

实验过程

A mixture of 5-(4-fluorophenyl)-4-(4-pyridyl)-2-(1H)-pyrimidinone (2.41 mmol) and phosphorus oxychloride (3 ml) was heated at reflux for 45 min. It was evaporated to dryness at a bath temperature of >500° C. The flask was cooled in an ice-bath and ice-water was added. If the pH value was found still acidic, then the mixture was neutralized with aqueous 5% ammonium hydroxide. It was extracted with dichloromethane, followed by washing of the organic solution with aqueous sodium chloride, drying and evaporation to yield the title compound as a yellowish foam which was used without further purification.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 45 min
  3. customIt was evaporated to dryness at a bath temperature of >500° C
  4. temperatureThe flask was cooled in an ice-bath
  5. additionice-water was added
  6. extractionIt was extracted with dichloromethane
  7. washby washing of the organic solution with aqueous sodium chloride
  8. customdrying
  9. customevaporation