反应详情

To a solution of 10.9 g (0.1 mole) of ethylchloroformate in 300 ml of anhydrous benzene is added dropwise, with stirring at room temperature, a solution of 14.5 g (0.05 M) of 11-(N-methyl-4-piperidylidene)-6,11-dihydro-5H-benzo-[5,6]-cyclohepta-[1,2-b]-pyridine (hereinafter referred to as Compound IA) in 200 ml of benzene. The solution is stirred and is heated under reflux overnight (16-20 hrs.). The mixture is cooled and is poured into ice water and the organic layer is separated, washed with water, dried, and then concentrated to dryness. The residue is triturated with petroleum ether and a white solid having a melting point of 106°-107° C. is recrystallized from isopropyl ether after decolorization with decolorizing carbon.

1. stirringThe solution is stirred
2. temperatureis heated
3. temperatureunder reflux overnight (16-20 hrs.)
4. temperatureThe mixture is cooled
5. customthe organic layer is separated
6. washwashed with water
7. customdried
8. concentrationconcentrated to dryness
9. customThe residue is triturated with petroleum ether
10. customis recrystallized from isopropyl ether after decolorization with decolorizing carbon