反应详情

{9-[(2R,3R,4S,5R)-3,4-Dihydroxy-5-(methoxymethyl)tetrahydro-2-furanyl]-6-[(2,2-diphenylethyl)amino]-9H-purin-2-yl}methyl methanesulfonate (300 mg, 0.53 mmol) (preparation 25) was dissolved in stirred dichloromethane (4 ml) and phenylmethanethiol (0.13 ml, 1.05 mmol) and triethylamine (0.15 ml, 1.05 mmol) added. The reaction mixture was stirred for 48 hr at room temperature and then the solvent removed under reduced pressure. The residue was partitioned between methanol (100 ml) and hexane (100 ml) and the methanol layer washed with a further amount of hexane (100 ml). The solvent was then removed under reduced pressure from the methanol layer. The residue was purified by column chromatography on silica gel eluting with a solvent system of ethyl acetate:hexane (3:2) increasing in polarity to ethyl acetate:methanol (98:2). This gave title compound (100 mg) as a foam. MS: 599 (MH+).

1. customthe solvent removed under reduced pressure
2. customThe residue was partitioned between methanol (100 ml) and hexane (100 ml)
3. washthe methanol layer washed with a further amount of hexane (100 ml)
4. customThe solvent was then removed under reduced pressure from the methanol layer
5. customThe residue was purified by column chromatography on silica gel eluting with a solvent system of ethyl acetate:hexane (3:2)
6. temperatureincreasing in polarity to ethyl acetate:methanol (98:2)