HRID4267

反应详情

EQUATION

反应方程式

HRID 4267 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Hydrogenate a mixture of 10% Pd/C (2.5 g), 10-phenyl-2,3-dihydroimidazo[1,2-a]pyrido[2,3-d]pyrimidin-5(10H)-one (5 g) and glacial acetic acid (125 ml) at 60 psi in a Paar apparatus for 24 hrs. at 25° C. Filter the mixture and evaporate the solvent of the filtrate. Dissolve the residue in 1N NaHCO3 (50 ml), neutralize with additional solid NaHCO3 and extract with CHCl3. Wash combined extracts with H2O, dry and filter. Evaporate solvent of the filtrate and crystallize the residue from EtOAc--MeOH to give 10-phenyl-2,3,6,7,8,9-hexahydroimidazo[1,2-a]-pyrido[2,3-d]pyrimidin-5(10H)-one, m.p. 248.0°-250.5° C.

WORKUP

后处理

  1. customat 25° C
  2. filtrationFilter the mixture
  3. customevaporate the solvent of the filtrate
  4. dissolutionDissolve the residue in 1N NaHCO3 (50 ml)
  5. extractionextract with CHCl3
  6. washWash
  7. customdry
  8. filtrationfilter
  9. customEvaporate solvent of the filtrate and crystallize the residue from EtOAc