Hydrochloric Acid → (3R)-Piperidin-3-amine--hydrogen chloride (1/2)

Temperature

26 °C

(R)-piperidine-3-amine dibenzoyl-D-tartrate (9.0 gm) and isopropanol (50 mL) were charged in a 500 mL round bottomed flask equipped with a mechanical stirrer and water (4.5 mL) was added. The mixture was stirred for 30 minutes at 26° C. and IPA.HCl (18%, 12 mL) was added and the resulted mixture was heated to 62° C. and maintained for 2 hours at 62° C. Reaction mixture was allowed to get 26° C. and stirred for 20 hours at 26° C. The precipitation formed was filtered and washed with 9 mL of IPA. The solid was dried under vacuum at 70° C. to get 2.1 gm of pure (R)-piperidine-3-amine dihydrochloride. Chiral Purity: 99.87%, (S)-isomer content: 0.13%.

1. customequipped with a mechanical stirrer
2. temperaturethe resulted mixture was heated to 62° C.
3. temperaturemaintained for 2 hours at 62° C
4. customReaction mixture
5. customto get 26° C.
6. stirringstirred for 20 hours at 26° C
7. customThe precipitation
8. customformed
9. filtrationwas filtered
10. washwashed with 9 mL of IPA
11. customThe solid was dried under vacuum at 70° C.

ORD record

ord-0ad6e26317d843f29dc7444adac3503d

Source dataset

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09056112B2