Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | D-Tartaric acid | HCID 439655 | — |
| Reactant | HCID 66759036 | HCID 66759036 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 57889970 | HCID 57889970 | 98% |
Reaction Steps
A suspension of (R)-4-(4-chlorophenyl)-3,3-dimethylpiperidin-4-ol, D-(−)-Tartaric Acid (6.2 g, 15.90 mmol) in concentrated hydrochloric acid (150 mL) was refluxed for 27 hours, during which time a clear solution was observed. The solution was cooled to 0° C., which caused a white solid to precipitate, and the pH was adjusted to ˜13 with the slow, careful addition of solid sodium hydroxide. The aqueous was extracted with EtOAc (3×300 mL), the combined organic layers were washed with 1N NaOH (3×100 mL), once with brine (100 mL), then dried over sodium sulfate and concentrated in-vacuo to yield the title compound (3.46 g, 15.60 mmol, 98% yield) as a pale yellow oil. MS (ESI+)=222/224, (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07601844B2 |
|---|
| Source dataset | uspto-grants-2009_10 |
|---|
| ORD ID | ord-0ec0218068fd46e294d817fe4ead5518 |
|---|
| Source note | uspto-grants-2009_10 |
|---|