HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromobenzene → (S)-1-Phenylpiperidine-3-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromobenzene | HCID 7961 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | 2-(Di-tert-butylphosphino)biphenyl | HCID 2734215 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Reactant | (3S)-piperidine-3-carboxylic acid hydrochloride | HCID 24820453 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Product | (S)-1-Phenylpiperidine-3-carboxylic acid | HCID 66743624 | — |
Reaction Steps
A mixture of bromobenzene (0.82 mL, 0.0078 mol), (3S)-piperidine-3-carboxylic acid hydrochloride (6.5 mmol, 0.0065 mol), sodium tert-butoxide (1.2 g, 0.013 mol), palladium acetate (40 mg, 0.0002 mol) and 2-(di-tert-butylphosphino)biphenyl (60 mg, 0.0002 mol) was degassed under vacuum and charged with nitrogen. To the mixture was added 1,4-dioxane (20 mL, 0.2 mol) and the resulting mixture was refluxed overnight. After cooling the reaction mixture to ambient temperature, the mixture was filtered and the filtrate was adjusted with TFA to pH=3.0 and extracted with EtOAc. The crude product was used in the following step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071624B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-41c51cd26d274050941f5faa7bdd9985 |
| Source note | uspto-grants-2011_12 |