2-amino-3,6-dimethylbenzonitrile

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 6 ml of concentrated hydrochloric acid were added to a solution of 5.84 g (0.04 mol) of 3,6-dimethylanthranilonitrile (Ib) in 80 ml of THF with stirring, after 15 min 5.6 g (0.04 mol) of dimedone (II) were added, the mixture was heated under reflux with stirring for 14 h, the precipitate was filtered off, washed with acetone and dried. The mother liquor was concentrated to 1/4 of the initial volume, the precipitate was filtered off, washed with acetone and dried. Precipitates were combined to give 10.5 g (87%) of IIId, m.p. 208-209 (i-PrOH). were added the mixture was heated under reflux the precipitate was filtered off washed with acetone dried The mother liquor was concentrated to 1/4 of the initial volume the precipitate was filtered off washed with acetone dried Precipitates to give 10.5 g (87%) of IIId, m.p. 208-209 (i-PrOH)