反応式
C[Si]([N-][Si](C)(C)C)(C)C.[Na+].[CH3:11][O:12][C:13](=[O:29])[CH2:14][C:15]1[CH:20]=[C:19]([C:21]([F:24])([F:23])[F:22])[CH:18]=[C:17]([C:25]([F:28])([F:27])[F:26])[CH:16]=1.[CH:30](I)([CH3:32])[CH3:31]>C1COCC1>[CH3:11][O:12][C:13](=[O:29])[CH:14]([C:15]1[CH:16]=[C:17]([C:25]([F:28])([F:26])[F:27])[CH:18]=[C:19]([C:21]([F:23])([F:24])[F:22])[CH:20]=1)[CH:30]([CH3:32])[CH3:31]参加物
5
反応条件
- 温度
- 0 °C
実験手順
Sodium bis(trimethylsilyl) amide (1.0M in THF—177 μL) was added drop-wise to a solution of (3,5-bis-trifluoromethyl-phenyl)-acetic acid methyl ester (389 mg) in dry THF (2 mL) at 0° C., under nitrogen atmosphere. After ten minutes, isopropyl iodide (143 μL) was added and the reaction mixture was stirred at 0° C. for 30 min. Further isopropyl iodide (143 μL) was added and the solution stirred at r.t. for 1 hour. The reaction was quenched with a 2N hydrochloric acid solution (2 mL) and the product was extracted with Et2O (2×). The combined organic extracts were dried and concentrated in vacuo to a residue which was purified by flash chromatography (CH/AcOEt 95:5) to give the title compound (184 mg) as a colourless oil.
後処理
- waitAfter ten minutes
- stirringthe solution stirred at r.t. for 1 hour
- customThe reaction was quenched with a 2N hydrochloric acid solution (2 mL)
- extractionthe product was extracted with Et2O (2×)
- customThe combined organic extracts were dried
- concentrationconcentrated in vacuo to a residue which
- customwas purified by flash chromatography (CH/AcOEt 95:5)
出典と根拠
- ORDレコード
- ord-be6c99b2b16b4f939114963e9941791e
- 出典データセット
- uspto-grants-2003_11
- 特許番号
- US06642240B2
関連ノート
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