反应详情

7 g of 1,2-dihydro-8-methoxy-4-methyl-1-oxo-5H-pyrido(4,3-b)indole is heated in 200 ml of phosphorus oxychloride at reflux for 3 days and the excess of oxychloride is evaporated off under reduced pressure. The residue is taken up in 100 ml of boiling water, the mixture is heated to boiling point for 3 minutes and filtered. The filtrate is alkalized cold with ammonia and the precipitate formed is separated, dried, then recrystallized from acetonitrile, giving 5.8 g of yellow micro-crystalls.

1. temperatureat reflux for 3 days
2. customthe excess of oxychloride is evaporated off under reduced pressure
3. temperaturethe mixture is heated
4. customfor 3 minutes
5. filtrationfiltered
6. customthe precipitate formed
7. customis separated
8. customdried
9. customrecrystallized from acetonitrile
10. customgiving 5.8 g of yellow micro-crystalls