참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanesulfonic Acid | HCID 6395 | — |
| 반응물 | 1-Ethyl-3-methoxy-2-pyridone-5-carbonitrile | HCID 21885851 | — |
| 반응물 | Sodium methanolate methanol | HCID 23694274 | — |
| 반응물 | (1s,2s)-1-(4-Fluorophenyl)-1-(6-fluoro-3-pyridyl)-1,2-propanediamine | HCID 44139477 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | HCID 178462509 | HCID 178462509 | 2.5% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06869966B2 |
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| 출처 데이터셋 | uspto-grants-2005_03 |
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| ORD ID | ord-c4b010fa84c74ceea0707d6a57c8fdde |
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| 출처 메모 | uspto-grants-2005_03 |
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