Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 3-Bromobenzonitrile | HCID 23381 | — |
| Reactant | tert-butyl (3S)-3-aminopyrrolidine-1-carboxylate | HCID 854071 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Catalyst | Binap, (A+-)- | HCID 634876 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66657313 | HCID 66657313 | 54.3% |
Reaction Steps
To a toluene solution (7 ml) containing 2.82 g of 3(S)-aminopyrrolidine-1-carboxylic acid tert-butyl ester (15 mmol) and 1.82 g of 3-bromobenzonitrile (10 mmol) were added 68.5 mg of BINAP (0.11 mmol), 22.5 mg of palladium acetate (0.1 mmol) and 3.91 g of cesium carbonate (12 mmol). The mixture was heated under reflux under a nitrogen atmosphere for 8 hours. After cooling to room temperature, water was added to the reaction solution, and extraction with dichloromethane was performed. After drying over sodium sulfate and concentration under reduced pressure, the residue was then purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1). The purified product was concentrated to dryness under reduced pressure to thereby obtain 1.56 g of light yellow powdery 3(S)-(3-cyanophenylamino)pyrrolidine-1-carboxylic acid tert-butyl ester.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08815871B2 |
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| Source dataset | uspto-grants-2014_08 |
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| ORD ID | ord-03b1685c27bf4a548ef5e6c2a299440d |
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| Source note | uspto-grants-2014_08 |
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