関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Fluoroaniline | HCID 9742 | — |
| 反応物 | Diethyl (ethoxymethyl)malonate | HCID 98702 | — |
| 溶媒 | 1,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene) | HCID 24670 | — |
| 生成物 | Ethyl 7-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate | HCID 178469609 | 67.6% |
反応手順
Under a nitrogen atmosphere, 3-fluoroaniline (50.0 g, 0.45 mol) and diethyl ethoxymethylmalonate (91 mL, 0.45 mol) were combined and heated at 100° C. for 3 hours. The reaction was allowed to cool to ambient temperature and it solidified. Dowtherm A (200 mL) was added and the reaction mixture was heated at 240° C. for 4 hours. The reaction mixture was allowed to cool to ambient temperature. The resulting precipitate was isolated by filtration, washed with hexane and then dried in a vacuum oven to provide 71.5 g of ethyl 7-fluoro-4-hydroxy-3-quinolinecarboxylate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06809203B2 |
|---|
| 出典データセット | uspto-grants-2004_10 |
|---|
| ORD ID | ord-634289ea48ee4766bd160165ae5e52f6 |
|---|
| 出典メモ | uspto-grants-2004_10 |
|---|
