関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Picolinic acid | HCID 1018 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | N-(3-fluoro-4-((methoxy(methyl)amino)carbonyl)phenyl)pyridine-2-carboxamide | HCID 23145523 | — |
| 反応物 | HCID 178448200 | HCID 178448200 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-(3-fluoro-4-(3-methyl-3-butenoyl)phenyl)pyridine-2-carboxamide | HCID 23145243 | — |
反応手順
9.89 ml of (2-methyl-2-propen-1-yl)magnesium chloride (0.50 M tetrahydrofuran solution) was added to a tetrahydrofuran (10 ml) solution of 500 mg of N-(3-fluoro-4-((methoxy(methyl)amino)carbonyl)phenyl)pyridine-2-carboxamide obtained in the same method as in Example 145 (step 3) or in accordance with the method or by combining it with an ordinary method but using pyridine-2-carboxylic acid, with cooling with ice. The reaction liquid was stirred for 3 hours with cooling with ice, and then water was poured into the reaction solution, extracted with ethyl acetate and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=3/1) to obtain the entitled compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728025B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-9581c41b61054aff8661bb529241a2ff |
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| 出典メモ | uspto-grants-2010_06 |
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