反应详情

Methyl-1-(2,3,5-tri-O-acetyl-β-L-ribofuranosyl)-1,2,4-triazole-3-carboxylate (62 g, 161 mmol) was placed in a steel bomb and treated with freshly prepared methanolic ammonia (350 ml, prepared by passing dry HCL gas into dry methanol at 0° C. until saturation) at 0° C. The steel bomb was closed and stirred at room temperature for 18 h. The steel bomb was then cooled to 0° C., opened and the content evaporated to dryness. The residue was treated with dry ethanol (100 ml) and evaporated to dryness. The residue obtained was triturated with acetone to give a solid, which was filtered and washed with acetone. The solid was dried overnight at room temperature and dissolved in a hot EtOH (600 ml) and water (10 ml) mixture. The volume of the EtOH solution was reduced to 150 ml by heating and stirring on a hot plate. The hot EtOH solution on cooling provided colorless crystals, which were filtered, washed with acetone and dried under vacuum. Further concentration of the filtrate gave additional material. The total yield was 35 g (89%).

1. customthe content evaporated to dryness
2. additionThe residue was treated with dry ethanol (100 ml)
3. customevaporated to dryness
4. customThe residue obtained
5. customwas triturated with acetone
6. customto give a solid, which
7. filtrationwas filtered
8. washwashed with acetone
9. customThe solid was dried overnight at room temperature
10. dissolutiondissolved in a hot EtOH (600 ml) and water (10 ml) mixture
11. temperatureby heating
12. stirringstirring on a hot plate
13. temperatureThe hot EtOH solution on cooling
14. customprovided colorless crystals, which
15. filtrationwere filtered
16. washwashed with acetone
17. customdried under vacuum
18. customFurther concentration of the filtrate gave additional material