反应详情

温度

160 °C

To a high pressure vial was added 3-(2-chloro-5-(trifluoromethyl)pyridin-4-ylamino)-N-methylpicolinamide (0.205 g, 0.62 mmol) and 5-aminoindolin-2-one (0.138 g, 1.2 eq) and n-BuOH (5 mL). HCl (˜1.25M HCl in ethanol, 0.5 mL, 1.0 eq) was added to the above mixture. The vial was sealed and heated at 160° C. with stirring overnight in an oil bath. The mixture was cooled to room temperature and concentrated under reduced pressure to obtain the crude. The crude was dissolved in EtOAc and washed with saturated NaHCO3 solution. The organic layers were concentrated and the crude was purified by silica gel chromatography (20%˜100% EtOAc/Hex). The product was precipitated from EtOAc and filtered to obtain the desired product as the free base (isolated yield 56%). The product was converted to the HCl salt.

1. customThe vial was sealed
2. temperatureThe mixture was cooled to room temperature
3. concentrationconcentrated under reduced pressure
4. customto obtain the crude
5. washwashed with saturated NaHCO3 solution
6. concentrationThe organic layers were concentrated
7. customthe crude was purified by silica gel chromatography (20%˜100% EtOAc/Hex)
8. customThe product was precipitated from EtOAc
9. filtrationfiltered