関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzoyl chloride | HCID 7412 | — |
| 反応物 | 3,4-Dimethylanisole | HCID 78411 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Lithium perchlorate | HCID 23665649 | — |
| 触媒 | Scandium(III) triflate | HCID 2734571 | — |
| 溶媒 | Nitromethane | HCID 6375 | — |
| 生成物 | (2-Methoxy-4,5-dimethylphenyl)(phenyl)methanone | HCID 23078360 | 93% |
反応手順
Commercially available 3,4-dimethylanisole (409 mg) was dissolved in nitromethane (6 ml) to prepare a solution. Lithium perchlorate (1.9 g) and benzoyl chloride (843 mg) were added to the solution, scandium trifluoromethanesulfonate (148 mg) was then added thereto, and the mixture was stirred at room temperature for 3 days. A saturated aqueous sodium hydrogencarbonate solution was added to the reaction solution, and the mixture was extracted with chloroform. The organic layer was washed with saturated brine, was dried over sodium sulfate and was concentrated. The residue was subjected to separation and purification by column chromatography on silica gel using hexane/ethyl acetate as a solvent to give (4,5-dimethyl-2-methoxyphenyl)(phenyl)methanone (667 mg, yield 93%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07560558B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-802b722db74e4c3998754ed0872a693d |
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| 出典メモ | uspto-grants-2009_07 |
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