反应详情

温度

65 °C

Treat a mixture of prop-1-en-2-yl(2-fluoro-4-methyl-5-(7-methyl-2-(methylamino)pyrido[2,3-d]pyrimidin-6-yl)phenyl)carbamate (1.09 g, 2.86 mmol) and 2-(1-(trifluoromethyl)cyclopropyl)ethanamine hydrochloride (0.542 g, 2.86 mmol) in THF (30 mL) with 1-methylpyrrolidine (1.52 mL, 14.3 mmol) and heat at 65° C. for 4 h. Cool the mixture to RT, dilute with EtOAc, wash with brine (2×), dry over MgSO4, concentrate to dryness and purify via silica gel chromatography (MeOH/EtOAc). Treat the resulting material with acetonitrile, cool to −20° C. for 2 h, collect the solids via filtration, rinse with acetonittrile (−20° C.) and dry to afford the title compound as a pale yellow solid (570 mg, 42% yield). MS (m/z): 477.2 (M+1).

1. additionTreat
2. temperatureCool the mixture to RT
3. washwash with brine (2×)
4. dry with materialdry over MgSO4
5. concentrationconcentrate to dryness
6. custompurify via silica gel chromatography (MeOH/EtOAc)
7. additionTreat the resulting material with acetonitrile
8. temperaturecool to −20° C. for 2 h
9. customcollect the solids
10. filtrationvia filtration
11. washrinse with acetonittrile (−20° C.)
12. customdry