反应详情

温度

100 °C

A mixture of 6-chloro-2-(5-nitropyridin-2-yl)-N-(2,2,2-trifluoroethyl)-5-(2,4,6-trifluorophenyl)pyrimidin-4-amine (101 mg, 0.22 mmol) and Iron powder (256 mg, 4.58 mmol) in 2 mL of methyl alcohol and 1 mL of acetic acid is heated at 100° C. for 1 h. The reaction mixture is cooled to room temperature and diluted with ethyl acetate. The organic layer is washed with saturated sodium bicarbonate and then with saturated sodium chloride, dried over magnesium sulfate, filtered, concentrated and dried under reduced pressure to yield 2-(5-aminopyridin-2-yl)-6-chloro-N-(2,2,2-trifluoroethyl)-5-(2,4,6-trifluorophenyl)pyrimidin-4-amine as a light yellow oil (100 mg). MS: m/z 434.2 (M+H). This product is used in the next step with out further purification.

1. temperatureThe reaction mixture is cooled to room temperature
2. washThe organic layer is washed with saturated sodium bicarbonate
3. dry with materialwith saturated sodium chloride, dried over magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customdried under reduced pressure