Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Formate | HCID 2723810 | — |
| Reactant | HCID 47265314 | HCID 47265314 | — |
| Reactant | HCID 178418416 | HCID 178418416 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86611467 | HCID 86611467 | 30% |
Reaction Steps
In a solution of 2.0 g of 4-bromo-2-methyl-N-(2-pyridylmethyl) benzoic acid amide in 20 ml of N,N-dimethylformamide in an autoclave, 0.67 g of sodium formate and 0.10 g of dichlorobis(triphenylphosphine) palladium (II) were added, and stirred under 1.05 MPa carbon monoxide atmosphere at 110° C. for 3 hours. After the completion of the reaction, the reaction mixture was left and cooled to room temperature, and poured in 100 ml of water, and extracted with ethyl acetate (50 ml ×2). The organic phases together were dehydrated with saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified with silica gel column chromatography that was eluated with ethyl acetate-hexane (9:1), and 0.50 g of the aimed product was obtained as pale yellow crystal.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08138213B2 |
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| Source dataset | uspto-grants-2012_03 |
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| ORD ID | ord-e02309bdee834e9a81082ccd3fc78765 |
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| Source note | uspto-grants-2012_03 |
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