Hydrazine → 4-Bromo-2-hydrazinylpyridine

Temperature

70 °C

To a solution of 4-bromo-2-fluoropyridine (2.0 g, 11.4 mmol) in pyridine (10 mL) was added hydrazine (5 mL, 159 mmol). The mixture was heated at 70° C. for 2 hours, then cooled to room temperature. The volatile organics were removed under reduced pressure, then water (60 mL) was added to the residue and an off-white solid precipitated. The solid was filtered, washed with water, and dried under reduced pressure at 50° C. to give 1.77 g (84%) of the title compound as an off-white solid. m/z (ES+) 188, 190 (M+H)+.

1. temperaturecooled to room temperature
2. customThe volatile organics were removed under reduced pressure
3. additionwater (60 mL) was added to the residue
4. customan off-white solid precipitated
5. filtrationThe solid was filtered
6. washwashed with water
7. customdried under reduced pressure at 50° C.

ORD record

ord-b576197fec684c52981498e594f1219b

Source dataset

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09428502B2