反応式
[I-].C[S+](C)(C)=O.[H-].[Na+].[CH3:9][N:10]1[C:14]([O:15][C:16]2[CH:21]=[C:20]([CH3:22])[CH:19]=[C:18]([O:23][CH2:24]/[CH:25]=[CH:26]/[C:27]([F:30])([F:29])[F:28])[N:17]=2)=[CH:13][C:12]([C:31]([F:34])([F:33])[F:32])=[N:11]1.O>CS(C)=O>[CH3:9][N:10]1[C:14]([O:15][C:16]2[CH:21]=[C:20]([CH3:22])[CH:19]=[C:18]([O:23][CH:24]=[CH:25][CH2:26][C:27]([F:30])([F:28])[F:29])[N:17]=2)=[CH:13][C:12]([C:31]([F:34])([F:32])[F:33])=[N:11]1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of trimethylsulfoxonium iodide (4.5 g, 20.5 mmol) in DMSO (50 ml) is added NaH (60% in oil, 0.82 g, 20.5 mmol) and the resulting mixture is stirred for 1 h at ambient temperature. To the resulting solution is added dropwise a solution of (E)-2-(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methyl-6-(4,4,4-trifluorobut-2-enyloxy)pyridine (example 1,7.1 g, 18.6 mmol) at 10° C. After 3 h of stirring at ambient temperature, the dark mixture is hydrolyzed with water (200 ml) and extracted 3 times with diethylether (50 ml). The organic fractions are washed with water, dried over anhydrous magnesium sulfate, filtered and evaporated in vacuo. Purification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v) yields the title compound (0.22 g, 3.1% yield) of m.p. 56° C.
後処理
- stirringAfter 3 h of stirring at ambient temperature
- extractionextracted 3 times with diethylether (50 ml)
- washThe organic fractions are washed with water
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- customevaporated in vacuo
- customPurification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v)
出典と根拠
- ORDレコード
- ord-d2471746428b47baab9624f8b8dea539
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06852673B2
関連ノート
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