反应详情

Compound 10.1 (390 mg, 0.774 mmol) was dissolved in 15 mL CH3CN, treated with 2,6-lutidine (0.3 mL, 2.59 mmol) and TMSBr (1.5 mL, 11.4 mmol). The mixture was stirred for 2 h and coevaporated with CH3CN under reduced pressure. The residue was treated with NH4OH (10 mL) and stirred at 45° C. for 1.5 h. The mixture was treated with 500 mg NaHCO3 and concentrated down under reduced pressure. The residue was subjected to reverse phase HPLC eluting with 0-25% CH3CN in water to yield compound 10.2 (220 mg, 73% yield). 1H NMR (D2O) δ 2.28 (m, 1H), 2.45 (m, 1H), 4.90 (m, 2H), 5.8 (m, 1H), 6.15 (m, 1H). 31P NMR (D2O) d 18.77. LRMS (ESI) MH+ C10H13N6O6P requires 345.2. Found 345.0.

1. stirringstirred at 45° C. for 1.5 h
2. concentrationconcentrated down under reduced pressure
3. washHPLC eluting with 0-25% CH3CN in water