関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-Cyano-4-methylpyridin-1-ium-1-olate | HCID 3725165 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Methylpyridine-2-carbaldehyde | HCID 10011894 | 14.8% |
反応手順
To a solution of 2-cyano-4-methylpyridine-N-oxide (3.29 g, 0.0279 mol) in 164 mL of methylene chloride at -78° C. was added 27.6 mL of DIBAL(H) and the mixture was stirred at -78° C. for 2 h. To the above mixture was added 13 mL of HCl (conc.) and 52 mL of water, and the mixture was warmed to room temperature. To the aqueous layer was added sodium bicarbonate solution, the solution was extracted with ether, and the combined organic layer was concentrated in vacuo. The residue was purified by chromatography on silica (ether) to afford 0.5 g (14.8%) of 4-methylpyridine-2-carboxaldehyde, as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05631264 |
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| 出典データセット | uspto-grants-1997_05 |
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| ORD ID | ord-e23f5702e9b34c30a8bfcc6c356b28a5 |
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| 出典メモ | uspto-grants-1997_05 |
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