関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | N-methoxy-N-methyl-2-methyl-6-trifluoromethyl-3-pyridinecarboxamide | HCID 86625530 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Methyl-6-(trifluoromethyl)nicotinaldehyde | HCID 28875322 | — |
反応手順
To a cooled (−78° C.) solution of N-methoxy-N-methyl-2-methyl-6-trifluoromethyl-3-pyridinecarboxamide (615 mg, 2.48 mmol) in THF (10 mL) was added lithium aluminum hydride (LAH, 1 N/THF, 1.23 mL). The mixture was stirred for 15 minutes, and then warmed to −10° C. After additional stirring for 30 minutes, the mixture was quenched with saturated potassium hydrogen sulfate solution (1 mL) and extracted with diethyl ether. The organic layer was dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure to give 2-methyl-6-trifluoromethyl-3-pyridinecarboxaldehyde quantitatively as oil. The crude product was used directly in the following reaction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07858621B2 |
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| 出典データセット | uspto-grants-2010_12 |
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| ORD ID | ord-adf0009457f64c29bc936bb352070a78 |
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| 出典メモ | uspto-grants-2010_12 |
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