Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | N-methoxy-N-methylquinoline-8-carboxamide | HCID 20803291 | — |
| Reactant | HCID 178418373 | HCID 178418373 | — |
| Solvent | Carbon Dioxide | HCID 280 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 8-Acetylquinoline | HCID 12208789 | 83% |
Reaction Steps
Quinoline-8-carboxylic acid methoxy-methyl-amide (2.16 g, 10 mmol) was dissolved in anhydrous THF (40 mL) and cooled to −78° C. The 3 M methyl magnesium iodide solution in diethyl ether (4.0 mL, 12 mmol, Aldrich) was slowly added to the reaction solution in dry ice bath. The reaction mixture was allowed to stir under nitrogen at room temperature for overnight then the reaction was cooled at ice bath and quenched with saturated aqueous ammonium chloride (40 mL). The organic phase was separated and the aqueous phase was extracted with ethyl acetate (30 mL×2). The combined organic layers were dried over anhydrous magnesium sulfate and concentrated via vacuo to give crude title compound as light yellow solid in 83% yield (1.42 g, 8.3 mmol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07196102B2 |
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| Source dataset | uspto-grants-2007_03 |
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| ORD ID | ord-272a937635c246c4857c604a74aae2bd |
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| Source note | uspto-grants-2007_03 |
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