反应详情

温度

80 °C

0.561 mL (11.57 mmol) of hydrazine monohydrate is added under nitrogen to a stirring solution of 1.09 g (3.86 mmol) of 2-chloro-6-(2,4-difluorophenylthio)nicotinonitrile in 15 mL of propanol. The reaction medium is heated at 80° C. for 4 hours. A precipitate is obtained when the reaction medium is returned to room temperature. This precipitate is filtered and rinsed with ethanol. The solid is dissolved in an ethyl acetate fraction and washed with a 1N HCl solution. The organic phase is dried on magnesium sulfate and dry evaporated to yield 420 mg (39%) of 6-(2,4-difluorophenylthio)-1H-pyrazolo[3,4-b]pyridin-3-amine in the form of a yellow solid.

1. customA precipitate is obtained when the reaction medium
2. customis returned to room temperature
3. filtrationThis precipitate is filtered
4. washrinsed with ethanol
5. dissolutionThe solid is dissolved in an ethyl acetate fraction
6. washwashed with a 1N HCl solution
7. customThe organic phase is dried on magnesium sulfate
8. customdry
9. customevaporated