反应详情

温度

110 °C

To a mixture of 6-chloro-5-(trifluoromethyl)pyridin-3-amine (200 mg, 1.018 mmol) in MeOH (3 mL) was added 6-chloro-5-(trifluoromethyl)pyridin-3-amine (200 mg, 1.018 mmol), NaHCO3 (171 mg, 2.035 mmol) and PdCl2(dppf) (74.5 mg, 0.102 mmol). The mixture was stirred under a N2 atmosphere at 110° C. for 30 min under microwave. Then the reaction residue was filtered and the solid was washed by MeOH. Then 6M HCl was added to the solution, which was stirred a rt for 1 h and then concentrated to give the crude product. The crude product was purified by preparative TLC (PE/EA=1:1, Rf=0.6) to yield a light yellow solid of 1-(5-amino-3-(trifluoromethyl)pyridin-2-yl)ethanone (120 mg, 0.500 mmol, 49.1% yield): 1H NMR (400 MHz, CD3OD) δ 8.10 (d, J=2.43 Hz, 1H), 7.30 (d, J=2.43 Hz, 1H), 2.56 (s, 3H); ES-LCMS m/z 205.0 (M+H).

1. filtrationThen the reaction residue was filtered
2. washthe solid was washed by MeOH
3. additionThen 6M HCl was added to the solution, which
4. stirringwas stirred a rt for 1 h
5. concentrationconcentrated
6. customto give the crude product
7. customThe crude product was purified by preparative TLC (PE/EA=1:1, Rf=0.6)