Acetic Acid → HCID 68812137, compound

Participants

Reaction Steps

To a mixture of 900 ml of toluene and 900 ml of THF were added 50.0 g (0.233 mole) of 2,6-diaminodibenzodioxin and 55.3 g (0.699 mole) of pyridine and 59.5 g (0.583 mole) of anhydrous acetic acid was added in drops to the mixture over a period of 10 minutes with stirring at room temperature. After the dropwise addition was over, the mixture was stirred overnight and a precipitate was recovered by filtration. The precipitate was submitted to reslurrying with toluene (250 ml×2) and then dried under reduced pressure to give 57.0 g (0.191 mole) of N,N′-diacetyl-2,6-diaminodibenzodioxin in an 82.0% yield. The product showed a purity of 99.3 area % (HPLC, 254 nm).

Provenance & Evidence