Hydrochloric Acid → 2-Fluoro-1-methyl-3-nitrobenzene

Temperature

140 °C

Cesium fluoride (97.5 g, 642 mmol) was added under nitrogen atmosphere to a solution of 2-chloro-1-methyl-3-nitrobenzene (73.4 g, 428 mmol) in DMSO (185 ml), and the mixture was stirred at 140° C. for 10 hours. The reaction mixture was then poured into 0.5N hydrochloric acid and extracted twice with ethyl acetate. The organic extract was washed with saturated saline and dried over magnesium sulfate. A crude product was obtained by vacuum concentration, and then purified by reduced-pressure distillation (boiling point: 118° C. to 122° C./15 mm Hg) to yield the title compound (54.4 g, 82%) as a yellow oil.

1. extractionextracted twice with ethyl acetate
2. extractionThe organic extract
3. washwas washed with saturated saline
4. dry with materialdried over magnesium sulfate
5. customA crude product was obtained by vacuum concentration
6. distillationpurified by reduced-pressure distillation (boiling point: 118° C. to 122° C./15 mm Hg)

ORD record

ord-cea43cac31684d89ae2ef4df3bbf113c

Source dataset

uspto-grants-2011_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07897792B2