HRID1532072

反应详情

EQUATION

反应方程式

HRID 1532072 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of N-[(E)-3-(3-methyl-4-oxo-1-n-propyl-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-6-yl)-4-n-propoxycinnamoyl]morpholine (0.5 g, 0.0011 mol) in ethanol (30 ml) was stirred with 10% palladium on charcoal catalyst (0.05 g) under a hydrogen pressure of 50 p.s.i. (3.45 bar) at room temperature for 14 hours. The reaction mixture was filtered and solvent removed by evaporation under vacuum. Trituration of the residue with diethyl ether, followed by crystallisation from ethyl acetate-hexane, afforded the title compound as white crystals (0.37 g, 74%), m.p. 132-133° C. Found: C, 64.39; H, 7.26; N, 14.80. C25H33N5O4 requires C, 64.22; H, 7.11; N, 14.98%.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. customsolvent removed by evaporation under vacuum
  3. customTrituration of the residue with diethyl ether, followed by crystallisation from ethyl acetate-hexane