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ChemicalBook CAS DataBase List (3-BROMO-PYRIDIN-2-YL)-HYDRAZINE

(3-BROMO-PYRIDIN-2-YL)-HYDRAZINE synthesis

2synthesis methods
-

Yield: 91%

Reaction Conditions:

with hydrazine in 1,4-dioxane at 20; for 15 h;Heating / reflux;

Steps:

1
To a solution of 2-chloro-3-bromopyridine (14.5 g, 75.1 mmol) in 100 mL of dioxane was added anhydrous hydrazine (35.4 mL, 1130 mmol) at RT. The reaction mixture was heated at reflux for 15 h, and then cooled to RT. After most of the solvent was removed under reduced pressure, the resulting residue was diluted with ethyl acetate, washed with water, dried over Na2SO4, and concentrated to provide a residue. Recrystallization of the residue in ethyl acetate and hexanes gave compound 1A (12.9 g, 91%) as a solid. LC/MS (m/z)=188 (M+H)+.

References:

Bristol-Myers Squibb Company US2009/93516, 2009, A1 Location in patent:Page/Page column 24