反应详情

温度

120 °C

(R)-tert-Butyl piperidin-3-ylcarbamate (1619 mg, 8.08 mmol) was added to a mixture of 5-chloro-4-fluoro-1H-pyrrolo[2,3-b]pyridin-3-amine (500 mg, 2.69 mmol; Example 8, Step D) and N-ethyl-N-isopropylpropan-2-amine (1408 μL, 8.08 mmol) in NMP (6.75 mL). N2 was bubbled through the mixture for 5 minutes, and the reaction was stirred at 120° C. under N2 for 24 hours. The mixture was allowed to cool, was diluted with 20% EtOAc/Et2O (200 mL) and washed with water (5×50 mL). The organic layer was then dried over MgSO4, filtered, and concentrated in vacuo to provide the crude (R)-tert-butyl 1-(3-amino-5-chloro-1H-pyrrolo[2,3-b]pyridin-4-yl)piperidin-3-ylcarbamate. LCMS (APCI+) m/z 366 (M+H)+.

1. customN2 was bubbled through the mixture for 5 minutes
2. temperatureto cool
3. additionwas diluted with 20% EtOAc/Et2O (200 mL)
4. washwashed with water (5×50 mL)
5. dry with materialThe organic layer was then dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo