Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Malonate | HCID 7761 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 66603271 | HCID 66603271 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66596895 | HCID 66596895 | 93% |
Reaction Steps
Sodium hydride (60% in oil) (0.39 g) was added under ice cooling to a THF solution (30 ml) of diethyl malonate (1.85 ml), and stirring was carried out until the generation of hydrogen stopped. 5-(3-Iodopropyl)-8-methoxy-1-methyl-2-oxo-1,2-dihydroquinoline (2.89 g) was added, followed by stirring at room temperature for 4.5 hours. The reaction mixture was added to cold hydrochloric acid, and extraction with dichloromethane was performed. After drying over anhydrous sodium sulfate, the dry product was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (dichloromethane:methanol=20:1). The purified product was concentrated under reduced pressure to thereby obtain 2.94 g (yield: 93%) of diethyl 2-[3-(8-methoxy-1-methyl-2-oxo-1,2-dihydroquinolin-5-yl)propyl]malonate as a yellow oil.
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-491b333abd33405c9b8ffe79ab3cc3db |
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| Source note | uspto-grants-2013_01 |
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