反应详情

A 2 mL microwave vial was charged with N-((6-(trifluoromethyl)pyridin-3-yl)methyl)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4-amine (50 mg, 0.16 mmol), 2,5-difluorobenzonitrile (130 mg, 0.97 mmol), acetonitrile (0.4 mL) and N,N-diisopropylethylamine (84 μL, 0.48 mmol). The mixture was subjected to microwave irradiation at 200° C. for 4 h. After cooling the mixture was diluted with chloroform (7 mL), and washed with 0.1 M NaH2PO4 (10 mL), dried (Na2SO4), filtered and concentrated. The residue was purified by semi-preparative HPLC (100×20.2 mm, C18 column; 20-90% MeCN/H2O [10 mM diethylamine]) to yield an off-white solid (8 mg).

1. customirradiation at 200° C. for 4 h
2. temperatureAfter cooling the mixture
3. washwashed with 0.1 M NaH2PO4 (10 mL)
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by semi-preparative HPLC (100×20.2 mm, C18 column; 20-90% MeCN/H2O [10 mM diethylamine])