Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Binap, (A+-)- | HCID 634876 | — |
| Reactant | 2-Butanamine, (S)- | HCID 6713753 | — |
| Reactant | HCID 86615001 | HCID 86615001 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 68817414 | HCID 68817414 | 90% |
Reaction Steps
Add 6-chloropyridine-2,4-dicarboxylic acid 2-ethyl ester 4-methyl ester (2.44 g, 10 mmol), palladium acetate (224 mg, 1.0 mmol), racemic-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (623 mg, 1.0 mmol), cesium carbonate (4.95 g, 15.2 mmol) in toluene (70 mL) in a sealed tube. Degas the tube for 5 min with nitrogen, add (S)-sec-butylamine (1.2 mL, 11.8 mmol) and seal the tube. Heat to 80° C. overnight. Cool to room temperature and filter the mixture through a filtering agent. Wash with ethyl acetate. Dissolve the solid in water and extract with ethyl acetate. Combine all organic solutions, concentrate and purify (silica gel chromatography, eluting with ethyl acetate and hexanes) to give the title compound (2.5 g, 90%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07618978B2 |
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| Source dataset | uspto-grants-2009_11 |
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| ORD ID | ord-e757c9781beb4e169984d37a7df28c59 |
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| Source note | uspto-grants-2009_11 |
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