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ChemicalBook CAS DataBase List 2,4-DICHLORO-5-NITROPYRIDINE
4487-56-3

2,4-DICHLORO-5-NITROPYRIDINE synthesis

6synthesis methods
-

Yield:4487-56-3 77%

Reaction Conditions:

with sulfuric acid;dihydrogen peroxide in water at 0 - 25; for 18 h;

Steps:

1 Synthesis of 2,4-dichloro-5-nitro-pyridine
Fuming H2SO4 (13 mL) was added dropwise to the stirred vessel. In a separate flask, concentrated H2SO4 was added to 4,6-dichloro-pyridin-3-ylamine (4.54 g, 27.9 mmol) and stirred until complete dissolution occurred. The amine solution was then added to the H2O2/fuming H2SO4 solution, dropwise. The reaction was allowed to warm to 25° C. over 18 h. The yellow solution was poured over ice and neutralized by the slow addition of solid NaHCO3. The resultant aqueous solution was extracted three times with EtOAc and the combined organic layers were dried (Na2SO4), decanted and concentrated to afford 2,4-dichloro-5-nitro-pyridine as a yellow solid (4.13 g, 77%).

References:

Boehringer Ingelheim International GmbH US2006/217417, 2006, A1 Location in patent:Page/Page column 13

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