関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Methyl 2-chloroquinoline-4-carboxylate | HCID 5202936 | — |
| 反応物 | 2,3,4,5-Tetrahydro-1H-benzo[c]azepine hydrochloride | HCID 17848794 | — |
| 触媒 | Tetrabutylammonium Iodide | HCID 67553 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Methyl 2-(1,3,4,5-tetrahydro-2H-2-benzazepin-2-yl)quinoline-4-carboxylate | HCID 71255482 | 43.9% |
反応手順
The mixture of 2-chloroquinoline-4-carboxylic acid methyl ester (3 g, 13.5 mmol), 2,3,4,5-tetrahydro-1H-2-benzazepine hydrochloride (3 g, 16.3 mmol), potassium carbonate (4.5 g, 32.6 mmol), tetrabutylammonium iodide (300 mg) and toluene (60 mL) was heated with stirring at 110° C. for 5 days. The solvent was removed under reduced pressure to give a residue which was purified by column chromatography on silica gel (ethyl acetate/petroleum ether, 1:4) to give 1.97 g of product as a yellow solid. MS obsd. (ESI+) [(M+H)+] 333.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08871756B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-19110ca4eced459bbf086d9bfde407b0 |
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| 出典メモ | uspto-grants-2014_10 |
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