反应详情

温度

80 °C

A mixture of bicyclo[1.1.1]pentan-1-ylamine (201 mg, 1.68 mmol), 6-amino-4-fluoronicotinonitrile (intermediate 21, 230 mg, 1.68 mmol) and diisopropylethylamine (1.47 ml, 8.39 mmol) in DMA (3 ml) was heated at 80° C. in a septum sealed reaction vessel for 48 h. The reaction mixture was heated for 5 h at 120° C. and 18 h at 80° C., then cooled, evaporated and purified twice by normal phase chromatography using 24 g RediSep® columns, eluting with gradients from heptane to EtOAc. Product containing fractions were combined and evaporated to give the title compound.

1. customsealed
2. customreaction vessel for 48 h
3. temperatureThe reaction mixture was heated for 5 h at 120° C. and 18 h at 80° C.
4. temperaturecooled
5. customevaporated
6. custompurified twice by normal phase chromatography
7. washeluting with gradients from heptane to EtOAc
8. additionProduct containing fractions
9. customevaporated