HRID326869

反应详情

EQUATION

反应方程式

HRID 326869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4.0 g (0.0169 mole) of 2-acetoxymethyl-7-hydroxy-4(3H)-pteridinone, 1.2 g (0.0214 mole) of potassium hydroxide and 5 ml of water in 80 ml of ethanol is refluxed for 4 hours. After cooling, the reaction mixture is filtered. The solid thereby isolated is washed with 30 ml of ethanol and taken up in 160 ml of water. The cloudy solution obtained is clarified by filtration and acidified with acetic acid to pH 3.6. The precipitate formed is isolated by filtration. It is purified by washing with ether and recrystallization from a mixture of ethanol and N,N-dimethylformamide. Yld: 2.0 g (61%), m.p. >300° C.

WORKUP

后处理

  1. temperatureis refluxed for 4 hours
  2. temperatureAfter cooling
  3. filtrationthe reaction mixture is filtered
  4. customThe solid thereby isolated
  5. washis washed with 30 ml of ethanol
  6. customThe cloudy solution obtained
  7. filtrationis clarified by filtration
  8. customThe precipitate formed
  9. customis isolated by filtration
  10. customIt is purified
  11. washby washing with ether and recrystallization from a mixture of ethanol and N,N-dimethylformamide