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HRID 2080463作成日:2026年10月26日
Diglycolamine → 2-[2-[5-Chloro-4-[(4-chlorophenylthio)(2,5-difluorophenyl)methyl]pyridin-2-ylamino]ethoxy]ethanol
https://huagongshe.com/reaction/2080463
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diglycolamine | HCID 13578 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | 2,5-Dichloro-4-[(4-chlorophenylthio)-(2,5-difluorophenyl)methyl]pyridine | HCID 23114567 | — |
| 溶媒 | Dichloromethane methanol | HCID 21226129 | — |
| 生成物 | 2-[2-[5-Chloro-4-[(4-chlorophenylthio)(2,5-difluorophenyl)methyl]pyridin-2-ylamino]ethoxy]ethanol | HCID 23114653 | 35% |
反応手順
A dioxane (1.5 ml) solution of the 2,5-dichloro-4-[(4-chlorophenylthio)(2,5-difluorophenyl)methyl]pyridine (210 mg, 0.504 mmol) obtained in Example 54 and 2-(2-aminoethoxy)ethanol (400 μl) was heated at 120° C. for 3 days in a sealed tube. The reaction mixture was cooled to room temperature and then, concentrated under reduced pressure. Water was added to the residue thus obtained, followed by extraction with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure. The residue thus obtained was subjected to silica gel column chromatography. The fraction obtained from the 30% methanol/methylene chloride eluate was concentrated under reduced pressure to give the title compound (85 mg, 0.175 mmol, 35%) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07932271B2 |
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| 出典データセット | uspto-grants-2011_04 |
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| ORD ID | ord-296c5fff487548418df8b5da8b434e9f |
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| 出典メモ | uspto-grants-2011_04 |
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