反応式
[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[C:7]([CH3:25])=[C:8]([C:16]([C:18]2[CH:19]=[N:20][N:21]([CH3:24])[C:22]=2[OH:23])=[O:17])[CH:9]=[CH:10][C:11]=1[S:12]([CH3:15])(=[O:14])=[O:13].C(N(CC)CC)C.[CH3:33][CH2:34][S:35][C:36](Cl)=[O:37].C(OCC)(=O)C>C1COCC1>[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[C:7]([CH3:25])=[C:8]([C:16]([C:18]2[CH:19]=[N:20][N:21]([CH3:24])[C:22]=2[O:23][C:36]([S:35][CH2:34][CH3:33])=[O:37])=[O:17])[CH:9]=[CH:10][C:11]=1[S:12]([CH3:15])(=[O:14])=[O:13]参加物
6
実験手順
The crude 5-hydroxy-1-methylpyrazol-4-yl 3-(2-methoxyethoxy)-2-methyl-4-(methylsulfonyl)phenyl ketone obtained in the same manner as the above step (3) was dissolved in anhydrous THF (10 mL), and triethylamine (190 mg) and 96% S-ethyl chlorothiolformate (151 mg) were added, followed by stirring for 1 hour at room temperature. Ethyl acetate (200 mL) was added to the reaction mixture, and the mixture was washed twice with a saturated brine. The organic layer was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:1) to obtain the desired product (250 mg).
後処理
- washthe mixture was washed twice with a saturated brine
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:1)
出典と根拠
- ORDレコード
- ord-8dc2054f3c8a477fb88d3c391353ef50
- 出典データセット
- uspto-grants-2013_06
- 特許番号
- US08466088B2
関連ノート
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