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ChemicalBook CAS DataBase List 2-Fluoro-4-nitrobenzoic acid
403-24-7

2-Fluoro-4-nitrobenzoic acid synthesis

3synthesis methods
A mixture of 2-fluoro4-nitrotoluene (31.1 g, 0.2 mol), tetrabutylammonium bromide (3.2 g,0.01 mol), 1.0 L of 1N NaOH, and KMnO4 (20.0 g) was stirred at room temperature. After 10 min, the resulting mixture was heated to 95 °Cwith stirring. Additional 30.0 g portions of KMnO 4 were added after 2 h and 3 h. After stirring at 95 °C for an additional 10 h, the reaction mixture was cooled to room temperature and filtered through Celite to remove MnO2. The filtrate was acidified to pH 2 by adding concentrated hydrochloric acid. An off-white precipitate formed that was collected by vacuum filtration. The crude solid was dissolved in 300 mL of 1N aqueous NaOH, acidified to pH 2 using concentrated hydrochloric acid, and the mixture extracted with CH 2 Cl 2 (3 × 200 mL). The combined CH2 Cl 2extracts were washed with 0.1 N aqueous HCl (2 × 100 mL), dried over anhydrous Na2SO4, and concentrated in vacuo to afford 27.3 g (73.7%)of 2-fluoro-4-nitrobenzoic acid as a white crystalline solid, m.p. 174.5–176.0 °C (lit 7. m.p. 176–177 °C)[1].
-

Yield:403-24-7 81%

Reaction Conditions:

with chromium(VI) oxide;periodic acid in acetonitrile; for 1 h;

Steps:

56

Periodic acid (1.69 g, 7.41 mmol) was dissolved in acetonitrile (25 mL) by vigorous stirring, and then chromium trioxide (0.16 g, 1.60 mmol) was dissolved into the solution. 2-Fluoro-4- nitrotoluene (0.33 g, 2.13 mmol) was added to the above solution with stirring. A white precipitate formed immediately with exothermic reaction. After 1 h of stirring, the supernatant liquid of the reaction mixture was decanted to a flask, and the solvent was removed by evaporation. The residues were extracted with methylene chloride (2x30 mL) and water (2x30 mL). The organic layer was dried over MgSO4, and concentrated to give 2-Fluoro-4-nitrobenzoic acid (Formula 37) (0.32 mg, 81%) as a white solid. 1HNMR δ 8.06 (ddd, 1 H, J=9.9, 2.2 and 0.3), 8.13 (ddd, 1 H, /=8.6, 2.2 and 0.9), 8.25 (ddd, 1 H,J=8.6, 7.0 and 0.3).

References:

WO2006/124118,2006,A1 Location in patent:Page/Page column 78

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