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ChemicalBook CAS DataBase List 2,6-Difluoro-3-nitropyridine
58602-02-1

2,6-Difluoro-3-nitropyridine synthesis

3synthesis methods
-

Yield: 74%

Reaction Conditions:

with nitric acid

Steps:

IV.a a
a 2,6-Difluoro-3-nitropyridine To a mixture of concentrated sulphuric acid (600 mL) and fuming nitric acid (90%, 400 mL) in a ice-bath (internal temperature maintained at 5-10° C.) was added drop-wise 2,6-difluoropyridine (200 g, 1.74 mol). The resulting mixture was stirred overnight at room temperature. The mixture was poured slowly into 3 kg of ice and extracted with Et2O (2*2 L). The combined organic layers were washed with aqueous 1.5 N NaOH (2*1 L), then with aqueous saturated NaHCO3 (400 mL) or until pH is around 8-9. The organic layers were dried over MgSO4, filtrated and concentrated under reduced pressure until constant weight (to remove unreacted 2,6-difluoropyridine: 10-12%). The title compound was obtained as a yellow liquid (207.3 g, 74% yield).

References:

Simoneau, Bruno US2002/28807, 2002, A1

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