反応式
[CH3:1][C:2]1[CH:6]=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([C:13]([F:16])([F:15])[F:14])=[CH:9][CH:8]=2)[S:4][C:3]=1[CH:17]=[O:18].C[Mg+].[Br-].[CH2:22](OCC)C>C1COCC1>[CH3:1][C:2]1[CH:6]=[C:5]([C:7]2[CH:8]=[CH:9][C:10]([C:13]([F:16])([F:14])[F:15])=[CH:11][CH:12]=2)[S:4][C:3]=1[CH:17]([OH:18])[CH3:22]参加物
5
実験手順
To a solution of 3-methyl-5-(4-Trifluoromethyl-phenyl)-thiophene-2-carbaldehyde (0.130 g, 0.481 mmole) in THF (5 mL), is injected 3.0 M MeMgBr in ethyl ether (0.27 mL, 0.810 mmole) dropwise. The reaction is stirred for 2 hours. The reaction is quenched with saturated NH4Cl(aq) (10 mL), then the aqueous solution is extracted with ethyl acetate (3×15 mL). The combined organic solution is washed with brine (3×50 mL), dried over Na2SO4 and concentrated. The crude product is purified on a silica gel column, eluting with 0-20% ethyl acetate in hexane and concentrated to provide the titled compound as yellow solid.
後処理
- customThe reaction is quenched with saturated NH4Cl(aq) (10 mL)
- extractionthe aqueous solution is extracted with ethyl acetate (3×15 mL)
- washThe combined organic solution is washed with brine (3×50 mL)
- dry with materialdried over Na2SO4
- concentrationconcentrated
- customThe crude product is purified on a silica gel column
- washeluting with 0-20% ethyl acetate in hexane
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-6c3090dad9ce47efa1756af0259d6d3c
- 出典データセット
- uspto-grants-2009_03
- 特許番号
- US07504433B2
関連ノート
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