Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Binap, (A+-)- | HCID 634876 | — |
| Reactant | tert-butyl (3S)-3-aminopyrrolidine-1-carboxylate | HCID 854071 | — |
| Reactant | 1-Bromo-2-chloro-3-methoxybenzene | HCID 23287864 | — |
| Reactant | Sodium t-butoxide | HCID 23676156 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 66657090 | HCID 66657090 | 77.9% |
Reaction Steps
To a 5 ml of toluene solution containing 0.20 g of 3(S)-aminopyrrolidine-1-carboxylic acid tert-butyl ester (1.1 mmol) and 0.238 g of 2-chloro-3-bromoanisole (1.1 mmol) were added 67.0 mg of BINAP (0.11 mmol), 24 mg of tris(dibenzylideneacetone)dipalladium (0.027 mmol) and 144 mg of sodium tert-butoxide (1.5 mmol). The mixture was heated under reflux under a nitrogen atmosphere at 100° C. for one hour. After cooling to room temperature, the reaction solution was filtered using Celite. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1→3:1). The purified product was concentrated to dryness under reduced pressure to thereby obtain 0.28 g of light yellow amorphous solid 3(S)-(3-chloro-4-methoxyphenylamino)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-e82f1a6885c54419b20f2aba66f7409f |
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| Source note | uspto-grants-2014_08 |
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