関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Amino-4-methylphenol | HCID 7264 | — |
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | 2-Pyridinecarboxaldehyde | HCID 14273 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178426743 | HCID 178426743 | 73% |
反応手順
To a slurry of 2-amino-4-methylphenol (4.40 g, 35.7 mmol) in 300 mL water, a water solution of pyridine-2-carbaldehyde (3.80 g, 35.5 mmol) was slowly added, forming a yellow slurry. After stirring overnight, the suspension was poured through a frit and the solid washed with water. The orange solid was dissolved in 300 mL CH2Cl2 and extracted with 3×100 mL water, dried over MgSO4 and filtered to give a red solution. The solvent was removed under vacuum to give a red oil. The oil was re-dissolved in CH2Cl2, layered with an equal volume of hexane and cooled to −35° C. to yield yellow crystals of 11(5.56 g, 73% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08530593B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-346124835bb6415c9c0a227b1352a1d6 |
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| 出典メモ | uspto-grants-2013_09 |
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