反应详情

9-(R)-2-phosphonomethoxypropyl)-2-amino-6-azidopurine (0.30 g, prepared according to Example 27) in 50% aqueous methanol (200 ml) containing hydrochloric acid (0.5 ml) was hydrogenated over 10% Pd/C (0.5 g) overnight at room temperature. The mixture was filtered, washed with water, filtrate alkalized with ammonia and evaporated in vacuo. The residue was deionized on a column of Dowex 50 X 8 (50 ml) (cf. Example 25) and the ammonia eluate evaporated to dryness. The residue in water (pH adjusted to 9) was applied on a column of Dowex 1 X 2 (acetate) which was first washed with water to remove salts and the product was then eluted with 1 M acetic acid. The fractions containing product were pooled, evaporated to dryness and codistilled with water (3×20 ml). The residue was crystallized from water (ethanol added to turbidity) to afford 9-(R)-2-phosphonomethoxypropyl)-2,6-diaminopurine (120 mg) identical with the preparation according to Example 19.

1. filtrationThe mixture was filtered
2. washwashed with water, filtrate
3. customevaporated in vacuo
4. customthe ammonia eluate evaporated to dryness
5. washwas first washed with water
6. customto remove salts
7. washthe product was then eluted with 1 M acetic acid
8. additionThe fractions containing product
9. customevaporated to dryness
10. customThe residue was crystallized from water (ethanol added to turbidity)