反应详情

In a 2000-ml three-necked flask that had been deaerated and filled with nitrogen were placed 50.69 g (0.2058 mole) of 3,3′-methylenediindole and 30.55 g (0.2061 mole) of triethyl orthoformate, then 640 g of methanol was added, and the mixture was stirred. To the mixture was added dropwise 5.0 g (0.0515 mole) of concentrated sulfuric over 3 minutes and the mixture was heated under reflux for 1 hour. The mixture was cooled to room temperature and the reddish brown crystals formed were collected by filtration and reslurried twice with 500 ml of methanol. The solvent was distilled off under reduced pressure and 36.81 g of solid C or indolo[3,2-b]carbazole (0.1438 mole, 69.9% yield) was obtained as a reddish brown powder.

1. customIn a 2000-ml three-necked flask that had been deaerated
2. additionfilled with nitrogen
3. additionTo the mixture was added dropwise 5.0 g (0.0515 mole) of concentrated sulfuric over 3 minutes
4. temperaturethe mixture was heated
5. temperatureunder reflux for 1 hour
6. customthe reddish brown crystals formed
7. filtrationwere collected by filtration
8. distillationThe solvent was distilled off under reduced pressure and 36.81 g of solid C