関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl 4-(1-hydroxybutyl)-3-methylbenzoate | HCID 68178586 | — |
| 触媒 | HCID 178418406 | HCID 178418406 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 4-butyryl-3-methylbenzoate | HCID 68157866 | 32.9% |
反応手順
To a solution of (+/−)-methyl 4-(1-hydroxybutyl)-3-methylbenzoate (0.8 g, 4 mmol) in dichloromethane (15 mL) was added manganese dioxide (3.13 g, 36.0 mmol). The reaction was stirred at 30° C. overnight. TLC showed starting material remained and the reaction was heated to reflux for 5 hours. The reaction was cooled to room temperature and filtered through Celite. The filtrate was concentrated and purified by flash column chromatography to give methyl 4-butyryl-3-methylbenzoate (290 mg) as an oil. 1H NMR (400 MHz, CDCl3, δ): 7.90 (d, J=7.6 Hz, 2H), 7.59 (d, J=7.6 Hz, 1H), 3.93 (s, 3H), 2.86 (t, J=7.6 Hz, 2H), 2.49 (s, 3H), 1.69-1.78 (m, 2H), 0.99 (t, J=7.6 Hz, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08859591B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-e9bac1529aae471cab60aa395555b6d3 |
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| 出典メモ | uspto-grants-2014_10 |
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