Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acrylic Acid | HCID 6581 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Tri-o-tolylphosphine | HCID 80271 | — |
| Reactant | HCID 57720160 | HCID 57720160 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 68845447 | HCID 68845447 | 26.5% |
Reaction Steps
2-(3-Bromobenzylamino)-1-(β-D-ribofuranosyl)-1H-benzimidazole (200 mg), acrylic acid (112 mg), palladium acetate (10 mg) and tri-o-tolylphosphine (28 mg) were suspended in acetonitrile (2 mL). To the mixture was added triethylamine (0.3 mL), and the mixture was stirred at 100° C. for 10 hours. The insoluble material was removed by filtration, and the solvent was removed under reduced pressure. The obtained residue was purified by preparative reverse phase column chromatography (Shiseido CAPSELL PAC C18UG80, 5 μm, 20×50 mm, flow rate 30 mL/minutes linear gradient, water/methanol=70/30-10/90) to give the title compound (52 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07547680B2 |
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| Source dataset | uspto-grants-2009_06 |
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| ORD ID | ord-a4efd77340a547239491cf4b0f3be1fb |
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| Source note | uspto-grants-2009_06 |
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