反应详情

A suspension of 1-(6-amino-9H-purin-9-yl)-3-(N-benzyloxycarbonyl-O-methyl-L-tyrosylamino)-1,3-dideoxy-β-D-ribofuranuronic acid (150 mg) prepared in Example 3 in water (200 ml) was adjusted to pH 3 with 1N hydrochloric acid. The resulting mixture was hydrogenated under medium pressure (3.0-3.5 atm.) over palladium black (30 mg) for 3 hours. The catalyst was removed by filtration and the filtrate was adjusted to pH 7 with 1N sodium hydroxide. The resulting mixture was concentrated under reduced pressure to a volume of 30 ml. The concentrate was applied to a column of non ionic adsorption resin "HP-20" (trade mark, Mitsubishi Chemical Industries, Ltd.) (50 ml) and the column was washed with water (100 ml) and then eluted with a mixture of methanol and water (3:7)(100 ml). The solvent was evaporated under reduced pressure and the residue was crystallized from 0.1N hydrochloric acid to give 1-(6-amino-9H-purin-9-yl)-1,3-dideoxy-3-(O-methyl-L-tyrosylamino)-β-D-ribofuranuronic acid dihydrochloride monohydrate (60 mg), mp. 215°-230° C. (dec.).

1. customThe catalyst was removed by filtration
2. concentrationThe resulting mixture was concentrated under reduced pressure to a volume of 30 ml
3. washthe column was washed with water (100 ml)
4. washeluted with a mixture of methanol and water (3:7)(100 ml)
5. customThe solvent was evaporated under reduced pressure
6. customthe residue was crystallized from 0.1N hydrochloric acid