HRID327055

反应详情

EQUATION

反应方程式

HRID 327055 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 5-(5-chloromethyl-2-n-propoxyphenyl)-1-methyl-3-n-propyl-1,6-dihydro-7H-pyrazolo[4,3-d]-pyrimidin-7-one (0.5 g, 0.0013 mol) in ethyl acetate (50 ml) was stirred with 10% palladium on charcoal catalyst under a hydrogen atmosphere at 50 p.s.i. and room temperature. After 1 hour, the mixture was filtered and the filtrate evaported under vacuum to give a pale green solid. Chromatography on silica gel (4 g) using a methanol in dichloromethane elution gradient gave a white solid, crystallisation of which from hexane-ethyl acetate gave the title compound as colourless needles (0.12 g, 26%), m.p. 115°-116° C. Found D,66.66; H,7.12; N,16.55. C19H24N4O2 requires C,67.04; H,7.11; N,16.46%

WORKUP

后处理

  1. customroom temperature
  2. filtrationthe mixture was filtered
  3. customto give a pale green solid
  4. washa methanol in dichloromethane elution gradient
  5. customgave
  6. customa white solid, crystallisation of which from hexane-ethyl acetate