関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Aniline | HCID 6115 | — |
| 反応物 | Diethyl (ethoxymethylene)malonate | HCID 6871 | — |
| 溶媒 | Diphenyl Ether | HCID 7583 | — |
| 生成物 | Ethyl 4-oxo-1,4-dihydroquinoline-3-carboxylate | HCID 220876 | 74.2% |
反応手順
31.7 g (147 mmol) of 2-Ethoxymethylene-malonic acid diethyl ester and 13.7 g (147 mmol) of aniline were stirred neat at 110° C. for 1 h, then 300 mL of diphenyl ether was added and the temperature of the oil bath was raised to 260° C. for 2 h. The solution was then cooled down to rt, diluted with 600 mL of hexanes and filtered. The solids were washed with 200 mL of hexanes and dried to yield 23.7 g of the product as a light brown powder. LC-MSD, m/z for C12H11NO3 [M+H]+=218.2, HPLC retention time: 2.5 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07557213B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-ff3561eb1b8246a19701c5c21e4103cc |
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| 出典メモ | uspto-grants-2009_07 |
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