関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Galactaric acid | HCID 3037582 | — |
| 反応物 | (4E)-N-Methyl-5-(3-pyridyl)-4-penten-2-amine | HCID 10219654 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | (4E)-N-Methyl-5-(3-pyridyl)-4-penten-2-amine Hemigalactarate | HCID 131722555 | — |
反応手順
(4E)-N-Methyl-5-(3-pyridyl)-4-penten-2-amine (1.60 g, 9.10 mmol) was dissolved in ethyl alcohol (20 mL), assisted by warming to 60° C. The warm solution was treated with galactaric acid (955 mg, 4.54 mmol) in one portion, followed by the dropwise addition of water (0.5 mL). The solution was filtered while hot to remove some insoluble material. The filtrate was allowed to cool to ambient temperature. The resulting crystals were filtered, washed with anhydrous diethyl ether, and dried under vacuum at 40° C. to yield 1.20 g (47.0%) of a white, crystalline powder, mp 148-150° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06979695B2 |
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| 出典データセット | uspto-grants-2005_12 |
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| ORD ID | ord-0bf00be2289647b3af150868dc494e11 |
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| 出典メモ | uspto-grants-2005_12 |
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