反应详情

温度

50 °C

113.0 g (292 mmol) 2-[4-(1-tert-butoxycarbonylpiperidin-4-yl)-butyl]-isoindol-1,3-dione are dissolved in 600 ml ethanol, added to 29.3 g (585 mmol) hydrazine hydrate and heated to boiling for three hours. After cooling the solution, the mixture is filtered and the filtrate is concentrated under vacuum. The residue is dispersed in the heat (ca. 50° C.) between 500 ml toluene and 500 ml 10% sodium hydroxide solution. The organic phase is washed once with 50 ml 10% sodium hydroxide solution and twice, each with 50 ml water. The solvent is removed under vacuum and the residue is dried at 70° C. under high-vacuum and processed further without additional purification. Yield of colorless oil: 64.0 g (85%).

1. temperatureheated
2. temperatureAfter cooling the solution
3. filtrationthe mixture is filtered
4. concentrationthe filtrate is concentrated under vacuum
5. additionThe residue is dispersed in the
6. washThe organic phase is washed once with 50 ml 10% sodium hydroxide solution
7. customThe solvent is removed under vacuum
8. customthe residue is dried at 70° C. under high-vacuum
9. customprocessed further without additional purification