反应详情

温度

23 °C

To a solution of the above 3-trifluoromethyl-pyridin-2-ylamine (16.21 g, 100 mmol) in acetonitrile (300 mL) at 5° C. was added NBS (17.8 g, 100 mmol) and the mixture was stirred at 23° C. for 1 h. Poured into ice and additional sat. NaHCO3-sol., extracted with EtOAc, washed with brine, dried over Na2SO4. Removal of the solvent in vacuum left a yellow solid, which was filtered through a silica gel and cotton wool column with dichloromethane to give the title compound as a yellow solid (23.71 g, 98%). MS (EI) 240.1 [(M)+], 242.0 [(M+2)+].

1. extraction, extracted with EtOAc
2. washwashed with brine
3. dry with materialdried over Na2SO4
4. customRemoval of the solvent in vacuum
5. waitleft a yellow solid, which
6. filtrationwas filtered through a silica gel and cotton wool column with dichloromethane