関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | Galactaric acid | HCID 3037582 | — |
| 反応物 | (2R)-(4E)-N-Methyl-5-(3-pyridyl)-4-penten-2-amine | HCID 9898976 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (2R)-(4E)-N-Methyl-5-(3-pyridyl)-4-penten-2-amine Hemigalactarate | HCID 131722556 | — |
反応手順
Galactaric acid (328.0 mg, 1.56 mmol) and (2R)-(4E)-N-methyl-5-(3-pyridyl)-4-penten-2-amine (600.0 mg, 3.40 mmol) were dissolved in 2-propanol (5 mL) and water (0.2 mL), assisted by heating and sonication. The hot solution was filtered to remove some insoluble material. The solvent was removed on a rotary evaporator, and the residue was dried under high vacuum, producing a cream-colored syrup. The syrup was dissolved in dry 2-propanol (5 mL) and cooled at 4° C. The resulting precipitate was filtered and dried under high vacuum to yield 700 mg (79.7%) of an off-white, crystalline powder, mp 131–134° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07045538B2 |
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| 出典データセット | uspto-grants-2006_05 |
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| ORD ID | ord-1a2a004ef5fa4e4bbba881568ee82f92 |
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| 出典メモ | uspto-grants-2006_05 |
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