反应详情

A mixture of (R)—N-(1-(6-(trifluoromethyl)pyridin-3-yl)ethyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine (300 mg, 0.93 mmol), 5-bromo-2-fluorobenzonitrile (560 mg, 2.8 mmol), N,N-diisopropylethylamine (480 μL, 2.8 mmol), and acetonitrile (4 mL) was subjected to microwave irradiation at 180° C. for 2 h. More 5-bromo-2-fluorobenzonitrile (500 mg) was added and the mixture was subjected to microwave irradiation at 180° C. for another 2 h. Additional 5-bromo-2-fluorobenzonitrile (500 mg) was added and the mixture was subjected to microwave irradiation at 180° C. for an additional 2 h. LC-MS indicated the amine was nearly completely consumed. After cooling the mixture was concentrated in vacuo, and the residue was purified by silica gel column (100% EtOAc) to yield a light yellow solid (255 mg, 54%).

1. customirradiation at 180° C. for 2 h
2. customirradiation at 180° C. for another 2 h
3. customirradiation at 180° C. for an additional 2 h
4. customwas nearly completely consumed
5. temperatureAfter cooling the mixture
6. concentrationwas concentrated in vacuo
7. customthe residue was purified by silica gel column (100% EtOAc)