関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1,1,1-Trifluoro-2-methylpropan-2-ol | HCID 68182 | — |
| 反応物 | 1-(Bromomethyl)-3-chlorobenzene | HCID 69838 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Chloro-3-(2,2,2-trifluoro-1,1-dimethylethoxymethyl)benzene | HCID 71287759 | — |
反応手順
To a suspension cooled to 0° C. of sodium hydride (126 mg, 60 wt. % oil dispersion) in N,N-dimethylformamide (5 ml) was added dropwise, 1,1,1-trifluoro-2-methylpropan-2-ol (320 μL) under argon atmosphere, and the mixture was stirred for 15 minutes. To this reaction mixture was added dropwise 1-bromomethyl-3-chlorobenzene (320 μL), and the mixture was stirred for 3 hours. To this reaction mixture was added water, and the mixture was extracted with ethyl acetate. This organic layer was washed with water and a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/0 to 40/1) to give the titled compound (389 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846746B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-8fa502f875ea4986a76c1d68f92ecf39 |
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| 出典メモ | uspto-grants-2014_09 |
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