Acetic Acid → HCID 22343609, compound

Participants

Reaction Conditions

Reaction Steps

1-Chloro-2,3-difluoro-5-nitrobenzene (3 g, 15.6 mmol) was added to acetic acid (10 mL) and methanol (250 mL). To this mixture was added iron powder (3.0 g) in portions, stirred for 2 h at 60-65° C., cooled to room temperature, and filtered. The filterate was stripped to a brown solid, which was extracted with ethyl acetate (3×200 mL), washed with 1N NaOH (3×100 mL), and brine (2×100 mL). The organic layer was dried over anhydrous magnesium sulfate, filtered and stripped down to yield the product as a pale yellow solid (2.6 g). Yield 100%; 1H NMR (400 MHz, CDCl3): δ 6.41 (m, 2 H), 3.65 (br s, 2 H) ppm.

Provenance & Evidence