Hydrochloric Acid → 4-Amino-2,6-dichloropyridine

Temperature

95 °C

To a solution of 2,6-dichloro-4-nitropyridine (14.82 g, 76.79 mmol) in 350 mL ethanol were sequentially added iron powder (19.91 g, 356.58 mmol), water (65.8 mL, 3.6 mol) and concentrated hydrochloric acid (14.1 mL, 464.1 mmol). After the reaction was performed by stirring for 16 h at 95° C., the reaction solution was cooled to room temperature, adjusted to neutral pH, and subjected to suction filtration. After the filtrate was concentrated, it was extracted with ethyl acetate. The organic phase was combined, dried with anhydrous MgSO4, and subjected to rotary evaporation to afford 11.9 g titled product with a yield of 95.1%.

1. temperaturethe reaction solution was cooled to room temperature
2. filtrationsubjected to suction filtration
3. concentrationAfter the filtrate was concentrated
4. extractionit was extracted with ethyl acetate
5. dry with materialdried with anhydrous MgSO4
6. customsubjected to rotary evaporation

ORD record

ord-b95c88575cab43939820d5159ff6f27a

Source dataset

uspto-grants-2014_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08680089B2