反应详情

A mixture of N-((6-methoxypyridin-3-yl)methyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine (350 mg, 1.3 mmol), 5-bromo-2-fluorobenzonitrile (640 mg, 3.2 mmol), N,N-diisopropylethylamine (0.67 mL, 3.9 mmol), and acetonitrile (4 mL) was subjected to microwave irradiation at 180° C. for 3 h. After that additional 5-bromo-2-fluorobenzonitrile (450 mg) was added and the mixture was subjected to microwave irradiation at 180° C. for another 2 h. After cooling, the mixture was diluted with EtOAc (100 mL) and washed with aq. Na2CO3 solution and brine, dried (Na2SO4) and concentrated. The residue was purified by silica gel column (EtOAc: 100%) to yield a light yellow solid.

1. customirradiation at 180° C. for 3 h
2. customirradiation at 180° C. for another 2 h
3. temperatureAfter cooling
4. washwashed with aq. Na2CO3 solution and brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. customThe residue was purified by silica gel column (EtOAc: 100%)
8. customto yield a light yellow solid