反应详情

温度

110 °C

To a solution of 4-chloro-3,5-difluoropicolinaldehyde (533 mg, 3.0 mmol) in n-BuOH (15 mL) was added hydrazine (0.113 mL, 3.60 mmol) and the reaction was heated at 110° C. for 22 hours. The reaction mixture was cooled, concentrated and the residue was dissolved in EtOAc (100 mL) and washed with saturated Na2CO3 solution, dried over Na2SO4, and evaporated to give a residue which was purified by silica gel column chromatography eluted with hexanes/EtOAc (0-100%) to give the title compound. MS [M+H] found 172.0.

1. temperatureThe reaction mixture was cooled
2. concentrationconcentrated
3. dissolutionthe residue was dissolved in EtOAc (100 mL)
4. washwashed with saturated Na2CO3 solution
5. dry with materialdried over Na2SO4
6. customevaporated
7. customto give a residue which
8. customwas purified by silica gel column chromatography
9. washeluted with hexanes/EtOAc (0-100%)