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-(Bromomethyl)-3-chlorobenzene | HCID 69838 | — |
| 反応物 | (2R)-1,1,1-trifluoropropan-2-ol | HCID 6993809 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Chloro-3-((R)-2,2,2-trifluoro-1-methylethoxymethyl)benzene | HCID 86680379 | 85% |
反応手順
Under argon atmosphere, a suspension of sodium hydride (77 mg, 60 wt % oil dispersion) in N,N-dimethylformamide (2.0 ml) was cooled to 0° C., a solution of (R)-1,1,1-trifluoropropan-2-ol (213 mg) in N,N-dimethylformamide (2.0 ml) was added thereto, and the mixture was stirred for 15 minutes. Then, a solution of 1-bromomethyl-3-chlorobenzene (311 mg) in N,N-dimethylformamide (2.0 ml) was added thereto, and then the mixture was stirred at room temperature for 2.5 hours. To this reaction mixture was added water, and the mixture was extracted with ethyl acetate. This organic layer was washed with a saturated aqueous solution of sodium chloride, dried over magnesium sulfate, and then concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (eluent: n-hexane/ethyl acetate=1/0 to 19/1) to give the titled compound (307 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-d36057139f1f4c4997e333649a93df93 |
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| 出典メモ | uspto-grants-2014_09 |
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