Potassium Carbonate → 1,3-Difluoro-5-methyl-2-nitrobenzene

Temperature

50 °C

A mixture of (3,5-difluoro-4-nitrophenyl)acetic acid (41 g), potassium carbonate (24.6 g) and DMF (205 ml) was slowly heated to about 50° C. for 30 minutes. The reaction was then cooled to about 25° C. and quenched into 2M HCl (1025 ml) and hexane (400 ml) and stirred for 10 minutes. The layers were separated and the aqueous layer was extracted with hexane (400 ml). The combined hexane layers were washed with saturated brine (2×200 ml), then dried with anhydrous sodium sulphate and the solution was concentrated to give the title compound as a low melting solid (26 g).

1. temperatureThe reaction was then cooled to about 25° C.
2. customquenched into 2M HCl (1025 ml) and hexane (400 ml)
3. customThe layers were separated
4. extractionthe aqueous layer was extracted with hexane (400 ml)
5. washThe combined hexane layers were washed with saturated brine (2×200 ml)
6. dry with materialdried with anhydrous sodium sulphate
7. concentrationthe solution was concentrated

ORD record

ord-d807456ec39f46a0af4d84c8278a90ac

Source dataset

uspto-grants-2013_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08481566B2