反应详情

温度

70 °C

To a solution of (1R,2S,3R,5R)-3-[(6-chloropyrimidin-4-yl)amino]-5-(hydroxymethyl)cyclopentane-1,2-diol (1.880 g, 7.239 mmol) in hydroiodic acid (23.9 mL) was added sodium iodide (5.42 g, 36.2 mmol). The mixture heated to 70° C. for 10 min then concentrated and azeotroped using toluene (3×). The residue was dissolved in acetone and NaHCO3 was added. The suspension was filtered and the filtrate was concentrated in vacuo to obtain the title compound (24 g, >99%). LC/MS: Rt=0.76 min ES+ 352 (FA standard).

1. concentrationthen concentrated
2. customazeotroped
3. dissolutionThe residue was dissolved in acetone
4. additionNaHCO3 was added
5. filtrationThe suspension was filtered
6. concentrationthe filtrate was concentrated in vacuo