Potassium Nitrate → 1-Chloro-2,5-difluoro-4-nitrobenzene

Temperature

0 °C

2-Chloro-1,4-difluorobenzene (1.34 mmol, 200 mg) was dissolved in concentrated sulphuric acid (1.7 ml) and cooled to 0° C.; KNO3 (1 eq., 1.34 mmol, 135 mg) was added in one lot and the mixture was stirred at 0° C. for 1 hour and at room temperature for 2 hours. The crude mixture was poured onto ice and extracted with ethyl acetate (2×); the organics were combined dried over Na2SO4, filtered and the solvent was evaporated to afford the title compound which was purified by chromatography (EtOAc n-hexane) to afford the title product, 228 mg, 88%, volatile oil under high vacuum.

1. extractionextracted with ethyl acetate (2×)
2. dry with materialthe organics were combined dried over Na2SO4
3. filtrationfiltered
4. customthe solvent was evaporated

ORD record

ord-4b666918e5c34b6394e75ce1e55deebc

Source dataset

uspto-grants-2012_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08288412B2