反应详情

A mixture of N-((6-(trifluoromethyl)pyridin-3-yl)methyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine (1.0 g, 3.2 mmol), 5-bromo-2-fluorobenzonitrile (0.97 g, 4.8 mmol), N,N-diisopropylethylamine (1.7 mL, 9.7 mmol), and acetonitrile (10 mL) was subjected to microwave irradiation at 180° C. for 2 h. More 5-bromo-2-fluorobenzonitrile (1.0 g) was added and the mixture was subjected to microwave irradiation at 180° C. for another 2 h. Then additional 5-bromo-2-fluorobenzonitrile (1.0 g) was added and the reaction mixture was subjected to microwave irradiation at 180° C. for an additional 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 (100% EtOAc) to yield a light yellow solid (0.90 g, 57%).

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. temperatureAfter cooling
5. washwashed with aq. Na2CO3 solution and brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated
8. customThe residue was purified by silica gel column (100% EtOAc)