反应详情

Anhydrous 3-aminopropyltriphenylphosphonium bromide hydrobromide, 9.0 g., is suspended in 30 ml. dry tetrahydrofuran and 0.038 moles of butyl lithium in heptane is added during 1 hour. After an additional 30 minutes, 3.44 g. of 9-chloro-11H-pyrrolo[2,1-b][3]benzazepin-11-one is added to the deep red solution and the reaction is maintained at reflux for 10 hours. Water, 500 ml., is added at room temperature and the solvent is removed in vacuo. The crude residue is treated with 10% hydrochloric acid until acidic (pH 2) and then 100 ml. benzene is added. After stirring, the benzene layer is removed by decantation and the remaining mixture is rendered basic with 10% sodium hydroxide solution and is extracted with 3 × 50 ml. portions of benzene. The benzene extracts are washed, then dried with anhydrous sodium sulfate and concentrated in a vacuum leaving a residue of 9-chloro-11-(3-aminopropylidene)-11H-pyrrolo[2,1-b][3]benzazepine.

1. temperaturethe reaction is maintained
2. temperatureat reflux for 10 hours
3. addition, is added at room temperature
4. customthe solvent is removed in vacuo
5. additionThe crude residue is treated with 10% hydrochloric acid until acidic (pH 2)
6. additionbenzene is added
7. customthe benzene layer is removed by decantation
8. extractionis extracted with 3 × 50 ml
9. washThe benzene extracts are washed
10. dry with materialdried with anhydrous sodium sulfate
11. concentrationconcentrated in a vacuum