反応式
[CH3:1][C:2](=[CH2:6])[CH2:3][Mg]Cl.O1CCCC1.[F:12][C:13]1[CH:14]=[C:15]([NH:25][C:26]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][N:29]=2)=[O:27])[CH:16]=[CH:17][C:18]=1[C:19](N(OC)C)=[O:20].N1C=CC=CC=1C(O)=O>O>[F:12][C:13]1[CH:14]=[C:15]([NH:25][C:26]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][N:29]=2)=[O:27])[CH:16]=[CH:17][C:18]=1[C:19](=[O:20])[CH2:3][C:2]([CH3:6])=[CH2:1]参加物
実験手順
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.
後処理
- customobtained in the same method as in Example 145 (step 3) or in accordance with the method
- temperaturewith cooling with ice
- customThe reaction liquid
- temperaturewith cooling with ice
- extractionextracted with ethyl acetate
- dry with materialdried with anhydrous sodium sulfate
- customThe solvent was evaporated away under reduced pressure
- customthe resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=3/1)
- customto obtain the entitled compound
出典と根拠
- ORDレコード
- ord-9581c41b61054aff8661bb529241a2ff
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07728025B2
関連ノート
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