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ChemicalBook CAS DataBase List 2,6-Difluoronitrobenzene
19064-24-5

2,6-Difluoronitrobenzene synthesis

7synthesis methods
-

Yield:19064-24-5 52%

Reaction Conditions:

with sodium perborate in acetic acid at 80 - 90; for 1 h;

Steps:

99.1
Step 1: A mixture of sodium perborate tetrahydrate (65 g, 422 mmol) in glacial acetic acid (250 mL) was stirred at 80° C. 2,6-Difluoroaniline (11.0 g, 85 mmol) in glacial acetic acid (50 mL) was added slowly to the mixture. The temperature was maintained between 80-90° C. for 1 hour. The cooled reaction mixture was poured into water and extracted twice with diethyl ether. The combined organic layers were washed with a dilute solution of sodium bicarbonate, dried over anhydrous magnesium sulfate and evaporated. The residue was purified via Biotage chromatography (FlasH90i, silica, 10% THF/hexane) and the product washed with hexane to afford 2,6-difluoronitrobenzene (7.0 g) (52%). MS (ESI) m/z 160 ([M+H]+).

References:

Wyeth US2005/222148, 2005, A1 Location in patent:Page/Page column 58

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