HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Bromide → Pregabalin
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Methyl ((S)-4-Methyl-2-[2-oxo-2-[[(S)-1-phenylethyl]amino]ethyl]pentyl]carbamate | HCID 59832562 | — |
| Solvent | Water | HCID 962 | — |
| Product | Pregabalin | HCID 5486971 | 90% |
Reaction Steps
A flask was loaded with 47% HBr (12 ml), water (6 ml), and compound 26 (6 g), and then was heated to reflux for 3 hours. The solution was cooled to room temperature, and water (12 ml) was added. An aqueous 47% sodium hydroxide solution was added to obtain pH of 3. The solution was then extracted twice with isobutanol (15 ml), the combined organic layers were evaporated and fresh isobutanol was added (15 ml). Bu3N (3.8 g) was added. The mixture was cooled to 2° C. for 1 hour, then (S)-Pregabalin was filtered, and washed with of iso-butanol (3 ml). After drying at 55° C. under vacuum, (S)-Pregabalin was obtained as white crystals in a 90% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07446220B2 |
| Source dataset | uspto-grants-2008_11 |
| ORD ID | ord-35c295d295db4a1bb0a36d318f83b824 |
| Source note | uspto-grants-2008_11 |