反应详情

A solution of 6-chloroadenosine (43 g) and cyclopentylamine (5 eq.) in ethanol (50 eq.) was heated at reflux for 3 hours then cooled to room temperature. The resultant reaction mixture was concentrated in vacuo and the resultant residue was diluted with water (400 ml) and ethyl acetate (400 ml). The eoganic layer was separated and the aqueous layer was extracted into ethyl acetate (2×400 ml). The combined organic layers were washed with water (2×200 ml), dried over sodium sulfate, concentrated in vacuo and dried under vacuum to provide a solid which was suspended in MeOH (400 mL), filtered and dried to provide N6-cyclopentyladenosine (43.8 g).

1. temperatureat reflux for 3 hours
2. customThe resultant reaction mixture
3. concentrationwas concentrated in vacuo
4. additionthe resultant residue was diluted with water (400 ml) and ethyl acetate (400 ml)
5. customThe eoganic layer was separated
6. extractionthe aqueous layer was extracted into ethyl acetate (2×400 ml)
7. washThe combined organic layers were washed with water (2×200 ml)
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated in vacuo
10. customdried under vacuum
11. customto provide a solid which
12. filtrationfiltered
13. customdried