HRID1700105

反应详情

EQUATION

反应方程式

HRID 1700105 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

10% w/w Palladium on carbon (200 mg) was added to a solution of (2R,3R,4R,5R)-4-(acetyloxy)-2-[(acetyloxy)methyl]-5-{2-cyano-6-[(2,2-diphenylethyl)amino]-9H-purin-9-yl}tetrahydro-3-furanyl acetate (Preparation 18) (1.9 g, 3.2 mmol) in ethanol saturated with ammonia (100 ml). The reaction mixture was stirred under an atmosphere of hydrogen 414 kPa (60 psi) for 16 hours at room temperature. The solids were removed by filtration through Arbocel (Trade Mark) and the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel eluting with dichloromethane:methanol:0.88 concentrated aqueous ammonia (90:10:1 by volume gradually changing to 80:20:2 by volume) to give the title compound as a solid (770 mg).

WORKUP

后处理

  1. customThe solids were removed by filtration through Arbocel (Trade Mark)
  2. customthe solvent was removed under reduced pressure
  3. customThe residue was purified by column chromatography on silica gel eluting with dichloromethane