反应详情

(3-{6-[6-(2-Morpholin-4-yl-ethylamino)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrazolo[3,4-d]pyrimidin-3-yl]-pyridin-2-ylamino}-3-phenyl-propyl)-carbamic acid tert-butyl ester (147 mg, 0.209 mmol) was dissolved in CF3COOH (4 mL). The mixture was heated at reflux for 15 hours. The solvent was removed under reduced pressure. A saturated aqueous solution of NaHCO3 was added to the residue, and then extracted with ethyl acetate (3×15 mL). The combined organic phase was dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. After purification by prep-HPLC, concentrated HCl was added to the fractions with product and concentrated under reduced pressure to give N1-{6-[6-(2-Morpholin-4-yl-ethylamino)-1H-pyrazolo[3,4-d]pyrimidin-3-yl]-pyridin-2-yl}-1-phenyl-propane-1,3-diamine; hydrochloride as a yellow solid. (Yield 16 mg, 16.2%).

1. temperatureThe mixture was heated
2. temperatureat reflux for 15 hours
3. customThe solvent was removed under reduced pressure
4. additionA saturated aqueous solution of NaHCO3 was added to the residue
5. extractionextracted with ethyl acetate (3×15 mL)
6. dry with materialThe combined organic phase was dried over anhydrous Na2SO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customAfter purification by prep-HPLC, concentrated HCl
10. additionwas added to the fractions with product
11. concentrationconcentrated under reduced pressure