反应详情

Triethylamine (0.2 ml, 1.14 mmol) was added to a stirred solution of (2R,3R,4R,5R)-4-(acetyloxy)-2-[(acetyloxy)methyl]-5-(6-chloro-2-cyano-9H-purin-9-yl)tetrahydro-3-furanyl acetate (500 mg, 1.14 mmol) (Preparation 45) and 2,2-bis(4-chlorophenyl)ethanamine (919 mg, 1.2 mmol) (J. Am. Chem. Soc., 1983, 105(10), 3138) in acetonitrile (5 ml) at room temperature. The reaction mixture was stirred for 16 hours. The solvent was then removed under reduced pressure and the residue was dissolved in dichloromethane (20 ml). The solution was washed with water (10 ml) and saturated sodium chloride solution (10 ml), dried over anhydrous magnesium sulphate and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel eluting with dichloromethane:methanol:(99:1 by volume) increasing in polarity to dichloromethane:methanol (98.5:1.5 by volume). The solvent was removed under reduced pressure to give the title compound (698 mg) as a foam.

1. customThe solvent was then removed under reduced pressure
2. dissolutionthe residue was dissolved in dichloromethane (20 ml)
3. washThe solution was washed with water (10 ml) and saturated sodium chloride solution (10 ml)
4. dry with materialdried over anhydrous magnesium sulphate
5. customevaporated under reduced pressure
6. customThe residue was purified by column chromatography on silica gel eluting with dichloromethane
7. temperaturemethanol:(99:1 by volume) increasing in polarity to dichloromethane:methanol (98.5:1.5 by volume)
8. customThe solvent was removed under reduced pressure