反应详情

12.8 g (29.2 mmol) 2-[3-(1-diphenylmethylpiperidine-4-yl)-propyl]-isoindol-1,3-dione are suspended in 110 ml ethanol and added to 2.2 ml (58.4 mmol) hydrazine hydrate and heated to boiling for three hours. After cooling, the mixture is concentrated under vacuum. The residue is dispersed between 300 ml dichloromethane and 50 ml 10% sodium hydroxide solution. The aqueous phase is extracted twice, each with 200 ml dichloromethane. The combined organic phases are washed twice, each with 20 ml water, and dried over sodium sulfate. The solvent is removed under vacuum and the residue is processed fruther without additional purification. Yield 7.3 g (81%)

1. temperatureheated
2. temperatureAfter cooling
3. concentrationthe mixture is concentrated under vacuum
4. additionThe residue is dispersed between 300 ml dichloromethane and 50 ml 10% sodium hydroxide solution
5. extractionThe aqueous phase is extracted twice
6. washThe combined organic phases are washed twice
7. dry with materialeach with 20 ml water, and dried over sodium sulfate
8. customThe solvent is removed under vacuum
9. customwithout additional purification