反应详情

A mixture of 2,5-dichloropyridine (7.4 g, 50 mmol) and 50 ml of hydrazine hydrate (1 mol) was refluxed for 3 hours and the mixture was diluted with ether. The crystalline solid (1st crop) was filtered, the solid was washed with water; and the aqueous layer was extracted with ether (2×). The organic layer was partially concentrated in vacuo and filtered to yield an additional white solid (2nd crop). The concentration of the filtrate yielded more solid (third crop). The combined solid product was dried in vacuo to afford 5.95 g (82%) of 2-hydrazino-5-chloropyridine as a white solid, m.p. 116°-122° C.

1. temperaturewas refluxed for 3 hours
2. filtrationThe crystalline solid (1st crop) was filtered
3. washthe solid was washed with water
4. extractionand the aqueous layer was extracted with ether (2×)
5. concentrationThe organic layer was partially concentrated in vacuo
6. filtrationfiltered
7. customto yield an additional white solid (2nd crop)
8. customThe concentration of the filtrate yielded more solid (third crop)
9. customThe combined solid product was dried in vacuo