関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzoyl chloride | HCID 7412 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Isoquinolin-5-ol | HCID 30386 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Benzoyloxyisoquinoline | HCID 23077393 | 103.6% |
反応手順
To a solution of 5-hydroxyisoquinoline (15.0 g, 103 mmol) in dichloromethane (300 ml) was added triethylamine (10.9 g, 108 mmol), and the mixture was cooled to 0° C. Under stirring, benzoyl chloride (15.2 g, 108 mmol) was added dropwise and the temperature was raised to room temperature. After stirring for 6 hours at room temperature, dichloromethane was added. The solution was washed with saturated aqueous solution of sodium hydrogencarbonate, then dried over anhydrous magnesium sulfate and solvent was distilled off, thereby affording 26.6 g of the title compound as a light brown liquid. Yield quantitative. 1H-NMR (DMSO-d6, δ): 7.68(2H, t, J=7.3 Hz), 7.75(1H, d, J=5.9 Hz), 7.79-7.85(3H, m), 8.12-8.16(1H, m), 8.28(2H, d, J=7.3 Hz), 8.55 (1H, d, J=5.9 Hz), 9.45(1H, s).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07425563B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-21ef90c8a9bb49ffb7cad4f0e5118f94 |
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| 出典メモ | uspto-grants-2008_09 |
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