反应详情

A solution of (-)-2-(2-amino-6-chlorpurin-9-ylmethyl)-1,4-butanediol (11.5 mg, 0.0423 mmol) in 50% aqueous formic acid (0.75 ml) was kept at 100° C./2 h and then evaporated to dryness, dissolved in 2 ml of water and lyophilized. The product was dissolved in 1 ml of water, 2 drops of conc. aqueous ammonia was added and the solution kept at 100° C. for 10 min, flushed with nitrogen to remove ammonia, and lyophilized. The residue was dissolved by warming with 1.2 ml of 20% aqueous methanol and the solution filtered and kept in open air to allow for slow partial evaporization of solvent. Crystalline needles were formed. Filtration, washing with 3 drops of water and drying yielded 6.4 mg (60%) of (-)-9-(4-hydroxy-2-hydroxymethylbutyl)guanine.

1. customwas kept at 100° C.
2. custom2 h
3. customevaporated to dryness
4. dissolutiondissolved in 2 ml of water
5. dissolutionThe product was dissolved in 1 ml of water
6. addition2 drops of conc. aqueous ammonia was added
7. customflushed with nitrogen
8. customto remove ammonia
9. dissolutionThe residue was dissolved
10. temperatureby warming with 1.2 ml of 20% aqueous methanol
11. filtrationthe solution filtered
12. customCrystalline needles were formed
13. filtrationFiltration
14. washwashing with 3 drops of water
15. customdrying