HRID979465

反应详情

EQUATION

反应方程式

HRID 979465 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 100 g of 4-phenyl-1(2H)-phthalazinone and 96.2 g of neopentylamine in 300 ml of p-xylene were added dropwise 83.7 g of phosphorus oxychloride with stirring and the resulting mixture was stirred under reflux for 4 hours. After allowing to be cooled, a saturated aqueous solution of NaHCO3 was added to the reaction mixture. Then, the mixture was extracted with chloroform and the organic layer was separated, dried and then concentrated. The residue was recrystallized from ethanol to afford the title compound as a pale yellow crystal. 100.8 g (Yield, 77%) Melting point: 215.5°-216.5° C.

WORKUP

后处理

  1. stirringthe resulting mixture was stirred
  2. temperatureunder reflux for 4 hours
  3. temperatureto be cooled
  4. extractionThen, the mixture was extracted with chloroform
  5. customthe organic layer was separated
  6. customdried
  7. concentrationconcentrated
  8. customThe residue was recrystallized from ethanol