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
10% 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 1) (1.9 g, 3.2 mmol) in a saturated solution of ammonia in ethanol (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 increasing to 80:20:2 by volume). This gave the title compound as a solid (770 mg).
WORKUP
后处理
- customThe solids were removed by filtration through Arbocel (Trade Mark)
- customthe solvent was removed under reduced pressure
- customThe residue was purified by column chromatography on silica gel eluting with dichloromethane