反应详情

7-(7H-Pyrrolo[2,3-d]pyrimidin-4-yl)-4,7-diaza-spiro[2.5]octane-4-sulfonic acid amide (intermediate 1) (1.95 mmol) was dissolved in dry DMF (15 ml), added Cs2CO3 (4.29 mmol), BOC2O (4.29 mmol) and stirred at rt for 16 h. The crude mixture was treated with water (150 mL) and extracted with EtOAc (3×100 mL). The combined organic phases were washed with H2O (2×50 mL), brine (2×50 mL), dried over Na2SO4, filtered and concentrated in vacuo. The product was purified by flash chromatography on silica using EtOAc in heptane as eluent.

1. extractionextracted with EtOAc (3×100 mL)
2. washThe combined organic phases were washed with H2O (2×50 mL), brine (2×50 mL)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe product was purified by flash chromatography on silica