Water → 2-Fluoroisonicotinic acid

Temperature

115 °C

20 g of 2-fluoro-4-methylpyridine was suspended in 500 mL of water, and 100 g of potassium permanganate was added thereto and stirred at 115° C. for 20 hours. The reaction solution was filtered through Celite while hot, and then the filtrate was concentrated under reduced pressure until the amount of the solvent became ⅓. The solution was neutralized with aqueous sodium hydroxide solution, and then aqueous hydrochloric acid solution was added thereto until its pH became 2. The formed white solid was taken out through filtration, and the filtrate was extracted twice with ethyl acetate, washed with saturated saline water and dried with sodium sulfate. The solvent was evaporated off under reduced pressure, and the resulting white solid was combined with the solid taken out through filtration to obtain 9.51 g of the entitled compound.

1. filtrationThe reaction solution was filtered through Celite while hot, and then the filtrate
2. concentrationwas concentrated under reduced pressure until the amount of the solvent
3. additionaqueous hydrochloric acid solution was added
4. filtrationThe formed white solid was taken out through filtration
5. extractionthe filtrate was extracted twice with ethyl acetate
6. washwashed with saturated saline water
7. dry with materialdried with sodium sulfate
8. customThe solvent was evaporated off under reduced pressure
9. filtrationtaken out through filtration

ORD record

ord-204ee269e00d43d3aa225d729aa8db58

Source dataset

uspto-grants-2010_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07855294B2