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Next, in an atmosphere of nitrogen, 0.64 g (28 mmoles) of metallic sodium was added in five portions to 90 ml of anhydrous methanol to prepare a methanolic solution of sodium methoxide. To the methanolic solution was added 10.2 g (57.3 mmoles) of 2,3-dicyanonaphthalene. While thoroughly stirring the mixture, anhydrous ammonia gas was bubbled into the mixture slowly over a period of about one hour at room temperature. Then, the mixture was heated under reflux for about 3 hours while bubbling anhydrous ammonia gas. After cooling the mixture, the deposited yellow-colored solid product was collected by filtration, thoroughly washed with methanol and dried in vacuum. Thus, about 9.5 g (86%) of 1,3-diiminobenzo(f)isoindoline was obtained as a yellow colored solid. It was used in the subsequent reaction without purification.

1. customwas bubbled into the mixture slowly over a period of about one hour at room temperature
2. temperatureThen, the mixture was heated
3. temperatureunder reflux for about 3 hours
4. customwhile bubbling anhydrous ammonia gas
5. temperatureAfter cooling the mixture
6. filtrationthe deposited yellow-colored solid product was collected by filtration
7. washthoroughly washed with methanol
8. customdried in vacuum