Sodium Chloride → 4-Hydrazinylpyridine dihydrochloride

Temperature

120 °C

4-Chloropyridine hydrochloride (14 g) was added to hydrazine monohydrate (50 mL) and the mixture was stirred at 120° C. for 1 hr. A 1 mol/L a aqueous sodium hydroxide solution (100 mL) and sodium chloride were added to the reaction solution. The mixture was extracted with ethyl acetate and the extract solution was dried and concentrated under reduced pressure. The residue was dissolved in ethyl acetate (100 mL) and 4 mol/L hydrochloric acid-ethyl acetate (50 mL) was added under ice-cooling. The precipitate was collected by filtration to give 4-hydrazinopyridine dihydrochloride (16 g) as a pale-yellow solid.

1. extractionThe mixture was extracted with ethyl acetate
2. customthe extract solution was dried
3. concentrationconcentrated under reduced pressure
4. dissolutionThe residue was dissolved in ethyl acetate (100 mL)
5. addition4 mol/L hydrochloric acid-ethyl acetate (50 mL) was added under ice-
6. temperaturecooling
7. filtrationThe precipitate was collected by filtration

ORD record

ord-fc31b835792442469be2e57c2892d74e

Source dataset

uspto-grants-2010_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07790725B2