反应详情

温度

40 °C

To a suspension of 2-([1,2,4]triazolo[4,3-a]pyridin-3-yl)-8-((4-fluoropiperidin-4-yl)methoxy)quinoline dihydrochloride (0.050 g, 0.111 mmol) and TEA (0.0619 mL, 0.444 mmol) in 0.4 mL THF, 0.3 mL dichloromethane, and 0.2 mL DMF was added 2-bromoacetamide (0.0184 g, 0.133 mmol). The reaction mixture was heated in a 40° C. reaction block and stirred 1 hour. The reaction mixture was cooled to ambient temperature, several drops of saturated NaHCO3 were added, and the milky mixture was heated back to 40° C. and stirred another 3 hours. The reaction mixture was cooled to ambient temperature, diluted with water, and the resulting solids were collected by vacuum filtration through a 0.2 micron nylon filter disc, rinsed with water, air dried, then washed successively with ethyl acetate, dichloromethane, and ether, air dried, and dried in vacuo to give the title compound (0.014 g, 0.0322 mmol, 29.0% yield) as a white powder. MS APCI (+) m/z 435 (M+1) detected.

1. customreaction block
2. temperatureThe reaction mixture was cooled to ambient temperature
3. temperaturethe milky mixture was heated back to 40° C.
4. stirringstirred another 3 hours
5. temperatureThe reaction mixture was cooled to ambient temperature
6. filtrationthe resulting solids were collected by vacuum filtration through a 0.2 micron nylon
7. filtrationfilter disc
8. washrinsed with water, air
9. customdried
10. washwashed successively with ethyl acetate, dichloromethane, and ether, air
11. customdried
12. customdried in vacuo