Ammonia → 4-Cyano-3-nitrobenzamide

Participants

Reaction Steps

2 g (9.71 mmol) Methyl 4-cyano-3-nitrobenzoate (Compound II-8) and 60 ml methanol were added into a reaction flask, stirred, and ammonia gas was passed through for 1 hour, then reacted for 8 hours at room temperature. After the reaction was completed, the mixture was concentrated under reduced pressure to evaporate most of the methanol. Then the mixture was extracted with 100 ml ethyl acetate, and the organic layer was washed with water for three times, dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrated to dryness to obtain 1.1 g (5.76 mmol) crude product, which was recrystallized from ethyl acetate-n-hexane to obtain 4-cyano-3-nitrobenzamide (compound I-8), 0.6 g, yield 32.6%.

Provenance & Evidence