Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1-(Bromomethyl)-4-chlorobenzene | HCID 69329 | — |
| Reactant | 2-Oxo-1,2-dihydroquinoline-4-carbaldehyde | HCID 285477 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86613915 | HCID 86613915 | 47% |
Reaction Steps
Sodium hydride (60% in oil) (1.3 g) was added at 0° C. to a DMF solution (50 ml) of 2-oxo-1,2-dihydroquinoline-4-carboxaldehyde (5.13 g), followed by stirring for 30 minutes. 4-chlorobenzylbromide (7.0 g) was added, and the resulting mixture was stirred at room temperature overnight. Water was added to the reaction mixture, extraction with ethyl acetate was performed, and the extract was dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:10→1:4). The purified product was recrystallized from a chloroform-diisopropyl ether-n-hexane mixed solvent to thereby obtain 4.13 g (yield: 47%) of 1-(4-chlorobenzyl)-2-oxo-1,2-dihydroquinoline-4-carboxaldehyde as a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08362252B2 |
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| Source dataset | uspto-grants-2013_01 |
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| ORD ID | ord-80692fda13f942a1903a7b61aabe859f |
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| Source note | uspto-grants-2013_01 |
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