反应详情

温度

25 °C

To a stirring solution of 3-[6-(7-Cyclopentyl-6-dimethylcarbamoyl-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino)-pyridine-3-carbonyl]-3,8-diaza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester (0.232 g, 1. mmol) in CH2Cl2 (4 mL) was added a solution of 4M HCl in dioxane (2.54 mL, 10.14 mmol, 10 eq) at 25° C. After 4 hours stirring at 25° C. the reaction mixture was filtered and washed with CH2Cl2 (5 mL). The residue was collected and taken up in water then basified with 1M NaOH and extracted with CH2Cl2 (2×15 mL). The combined organic layers were dried over Na2SO4, filtered, and concentrated under reduced pressure to a tan solid. The crude was purified using Column Chromatography (MeOH/CH2Cl2) giving the desired product as a white solid (0.290 g, 0.594 mmol, 59%).

1. filtrationwas filtered
2. washwashed with CH2Cl2 (5 mL)
3. customThe residue was collected
4. extractionextracted with CH2Cl2 (2×15 mL)
5. dry with materialThe combined organic layers were dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure to a tan solid
8. customThe crude was purified