HRID217885

反应详情

EQUATION

反应方程式

HRID 217885 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3.2 g (8.59 mmol) of (+/−)2-(4-oxo-2-pyridin-4-yl-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidin-9-yl)-1H-isoindole-1,3(2H)-dione dissolved in 24 mL of ethanol was added 2.09 mL (43 mmol) of hydrazine hydrate and the resulting mixture was stirred under reflux for 2 h. The mixture was filtered and the solid obtained was triturated with dichloromethane for 24 h, filtered, and the resulting filtrates were evaporated to dryness. The resulting residue was purified on silica gel eluting with a mixture of dichloromethane/methanol in the proportions 98/2 to 96/4 to give 1.37 g (66%) of the desired compound as a brown powder.

WORKUP

后处理

  1. temperatureunder reflux for 2 h
  2. filtrationThe mixture was filtered
  3. customthe solid obtained
  4. customwas triturated with dichloromethane for 24 h
  5. filtrationfiltered
  6. customthe resulting filtrates were evaporated to dryness
  7. customThe resulting residue was purified on silica gel eluting with a mixture of dichloromethane/methanol in the proportions 98/2 to 96/4