HRID4267
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customat 25° C
- filtrationFilter the mixture
- customevaporate the solvent of the filtrate
- dissolutionDissolve the residue in 1N NaHCO3 (50 ml)
- extractionextract with CHCl3
- washWash
- customdry
- filtrationfilter
- customEvaporate solvent of the filtrate and crystallize the residue from EtOAc