反应详情

温度

100 °C

A mixture of the product from step (iv) (0.1 g), 2-amino-3-bromo-5-methylpyridine (0.071 g), tetrakis(triphenylphosphine)palladium(0) (0.046 g), sodium carbonate (0.12 g) in methanol (2 ml) was heated in a CEM microwave (variable wattage up to 150 W) at 100° C. for 10 min. The mixture was loaded onto SCX resin (sulphonic acid resin), flushed with methanol then the product eluted with methanol/ammonia. The methanol/ammonia filtrate was evaporated under reduced pressure then loaded onto bondelut-NH2 resin. The resin was flushed with methanol then the product eluted with methanol/acetic acid. The methanol/acetic acid filtrate was evaporated and the residue purified by RPHPLC. Yield 0.089 g

1. customflushed with methanol
2. washthe product eluted with methanol/ammonia
3. customThe methanol/ammonia filtrate was evaporated under reduced pressure
4. customThe resin was flushed with methanol
5. washthe product eluted with methanol/acetic acid
6. customThe methanol/acetic acid filtrate was evaporated
7. customthe residue purified by RPHPLC