reactants are commercially availlable.
zhao, qian, wo2010/22076, a1, (2010) 2-chloro-5- fluoropyridine (5.00 g, 38.01 mmol) was combined with hydrazine monohydrate (15 ml, 303.0 mmol) in a teflon.(r). lined reactor. the reaction was purged with argon gas and sealed, then heat ed to 200 0c overnight. following overnight heating, the reaction mixture was evaporated to solids under reduced pressure, and then dissolved in water containing nahco3. the mixture was transferred to a separatory funnel, and extracted 4 times with etoac. the combined organic extracts were dried over na2so4, filtered and concentrated to residue under reduced pressure, followed by purification by f lash column chromatography eluting with 5percent meoh 0.5percent nh4oh in dcm to give the desired 5-fluoro-2-hydrazinylpyridine (1.50 g, 31percent yield). ms apci ( ) m/z 128.0 (m l) detected.
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