反应详情

温度

27.5 °C

In a clean round bottom flask, 100 ml acetic acid, 50 gms 3-(R)-aminopiperidine dihydrochloride & 56.5 gms of 4-methylphthalic anhydride were charged. The reaction mass was refluxed & then cooled to 25-30° C. Acetone was added to the reaction mass & obtained solid was filtered. Acetone was added to the solid obtained & refluxed to get uniform slurry. The reaction mass was cooled to 25-30° C. & filtered. Wet wt 70 gms. In another round bottom flask, methylene dichloride, wet cake and water were charged. The reaction mass was basified & layers were separated. The organic layer was washed with water & concentrated upto half volume. Diisopropyl ether was added to the reaction mass to obtain the product. Dry wt 40 gms, HPLC purity=85%

1. temperatureThe reaction mass was refluxed
2. customobtained solid
3. filtrationwas filtered
4. additionAcetone was added to the solid
5. customobtained
6. temperaturerefluxed
7. customto get uniform slurry
8. temperatureThe reaction mass was cooled to 25-30° C.
9. filtrationfiltered
10. additionIn another round bottom flask, methylene dichloride, wet cake and water were charged
11. customlayers were separated
12. washThe organic layer was washed with water
13. concentrationconcentrated upto half volume
14. additionDiisopropyl ether was added to the reaction mass
15. customto obtain the product
16. customDry