反应详情

A mixture of tert-butyl 1-(6-fluoro-3,4-di(pyridin-2-yl)quinolin-2-yl)ethylcarbamate (0.4146 g, 0.933 mmol) was dissolved in hydrochloric acid, 4 M solution in 1,4-dioxane (4.66 mL, 18.65 mmol) and the mixture was stirred at rt. After 3.5 h, the mixture was partitioned between DCM (50 mL) and water (50 mL). The acidic aq mixture was washed with DCM (30 mL×2) to remove organic impurities and then basified to ˜pH 10 with 10 N NaOH (3.5 mL), extracted with DCM (50 mL×3). The combined organic layers were washed with water (100 mL×1), brine (100 mL×1), dried over MgSO4, filtered, and concentrated in vacuo to give 1-(6-fluoro-3,4-di(pyridin-2-yl)quinolin-2-yl)ethanamine as an orange syrup: LC-MS (ESI) m/z 345.1 [M+H]+. The orange syrup was carried on crude without further purification.

1. customthe mixture was partitioned between DCM (50 mL) and water (50 mL)
2. washThe acidic aq mixture was washed with DCM (30 mL×2)
3. customto remove organic impurities
4. extractionextracted with DCM (50 mL×3)
5. washThe combined organic layers were washed with water (100 mL×1), brine (100 mL×1)
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo