関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | 1-Ethyl-3-methoxy-2-pyridone-5-carbonitrile | HCID 21885851 | — |
| 反応物 | Sodium methanolate methanol | HCID 23694274 | — |
| 反応物 | (1s,2s)-1-(4-Fluorophenyl)-1-(6-fluoro-3-pyridyl)-1,2-propanediamine | HCID 44139477 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178462509 | HCID 178462509 | 2.5% |
反応手順
1-ethyl-3-methoxy-2-pyridone-5-carbonitrile (30 mg) was dissolved in methanol (1 mL), and 25% sodium methoxide-methanol solution (6.6 mL) was added thereto. The mixture was stirred at room temperature for 17 hours, and methanesulfonic acid (11 μL) and a solution of (1S,2S)-1-(4-fluorophenyl)-1-(6-fluoro-3-pyridyl)-1,2-propanediamine (44.5 mg) in methanol (1 mL) were successively added. The mixture was stirred at room temperature for two days and concentrated in vacuo. The residue was dissolved in ethyl acetate, and the solution was washed with brine, and dried over anhydrous sodium sulfate. After removal of the sodium sulfate by filtration, the organic solvent was evaporated in vacuo to give a residue, which was purified by column chromatography on silica gel (chloroform:methanol=10:1) to give the title compound (1.8 mg) as a brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07138525B2 |
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| 出典データセット | uspto-grants-2006_11 |
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| ORD ID | ord-c39a232061f34db6a09e694396fbca9a |
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| 出典メモ | uspto-grants-2006_11 |
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