Acetone → 3-(R)-(4-Methylphthalimido)piperidine

Temperature

5 °C

In a clean round bottom flask, 1000 ml methanol and 200 gm 3-(R)-aminopiperidine dihydrochloride were charged. Cooled the reaction mass to 0-10° C. and added 1850 ml 2.5% methanolic NaOH solution slowly at 0-10° C. Stirred and filtered the inorganic solid, distilled out clear filtrate under vacuum below 45° C. Added 400 ml acetic acid and cooled the reaction mass to room temperature, added 226.1 gm 4-methylphthalic anhydride. Reaction mass was refluxed & then cooled to 25-30° C. Acetone was added to the reaction mass & obtained solid was filtered. Acetone was again added to the solid obtained & refluxed to get uniform slurry. The reaction mass was cooled to 25-30° C. & filtered. Dry wt: 280 gms.

1. filtrationfiltered the inorganic solid
2. distillationdistilled out clear filtrate under vacuum below 45° C
3. additionAdded 400 ml acetic acid
4. temperaturecooled the reaction mass to room temperature
5. additionadded 226.1 gm 4-methylphthalic anhydride
6. customReaction mass
7. temperaturewas refluxed
8. temperaturecooled to 25-30° C
9. customobtained solid
10. filtrationwas filtered
11. additionAcetone was again added to the solid
12. customobtained
13. temperaturerefluxed
14. customto get uniform slurry
15. temperatureThe reaction mass was cooled to 25-30° C.
16. filtrationfiltered
17. customDry

ORD record

ord-890dd83a095640659b393927c2894b51

Source dataset

uspto-grants-2016_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09353114B2