Acetic Anhydride → 3-Cyanobenzoic acid

Participants

Reaction Steps

Acetic acid (30 ml), acetic anhydride (70 ml), sodium acetate (6.2 g), and m-cyanobenzamide (5.0 g) were mixed with stirring under cooling with ice, to thereby obtain a mixture. The mixture was allowed to react while the mixed gas of nitrogen monoxide and nitrogen dioxide (volume ratio 1:1) was introduced thereto at 286 N ml/minute for four hours. The residual solvent was removed through distillation in vacuum, and water was added to the residue, to thereby form crystals. The precipitated crystals were collected through filtration, washed with water, and dried, to thereby obtain 4.78 g of m-cyanobenzoic acid (yield 94%, based on m-cyanobenzamide). The m-cyanobenzoic acid obtained had a purity of 98%.

Provenance & Evidence