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ChemicalBook CAS DataBase List 3-chloro-2,6-difluoropyridin-4-aMine
405230-78-6

3-chloro-2,6-difluoropyridin-4-aMine synthesis

5synthesis methods
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Yield:405230-78-6 72%

Reaction Conditions:

with palladium 10% on activated carbon;hydrogen in ethanol;water at 50; under 3750.38 Torr; for 2 h;

Steps:

1 Synthesis of 4-amino-3-chloro-2,6-difluoropyridine:

40g 4-amino-3,5-dichloro-2,6-difluoropyridine, 43g potassium phosphate, 2g10% palladium-carbon catalyst (water content 54%) and 200mL50%The ethanol aqueous solution was added to the hydrogenation kettle and replaced with nitrogen and hydrogen in sequence.Then, the reaction was stirred at 50°C under 0.5MPa hydrogen pressure for 2h, and then cooled to room temperature.Most of the solvent was evaporated under reduced pressure, and a large amount of solid was precipitated, diluted with 100 mL of water, and filtered with suction.The filter cake was thoroughly washed with water, and then recrystallized with 20 mL of 50% ethanol aqueous solution,Obtained 23.6 g of white needle-like solid, which is 4-amino-3-chloro-2,6-difluoropyridine,The HPLC content is 98.5%, and the yield is 72%.

References:

CN112321497,2021,A Location in patent:Paragraph 0021; 0025