関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Isobutyronitrile | HCID 6559 | — |
| 反応物 | 2-Chloro-5-fluoroanisole | HCID 2724520 | — |
| 反応物 | Potassium bis(trimethylsilyl)amide | HCID 3251421 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(4-Chloro-3-methoxyphenyl)-2-methylpropanenitrile | HCID 17989155 | 31% |
反応手順
1-Chloro-4-fluoro-2-methoxy-benzene (4.3 g, 26.78 mmol) and isobutyronitrile (9.61 mL, 4.0 eq.) were dissolved in toluene (9.0 mL), added with KHMDS (80 mL, 0.5 M toluene solution) and stirred at 65° C. for 2 hr. The reaction solution was cooled to room temperature, added with aqueous solution of 1 N hydrochloric acid and then extracted with MTBE. The organic layer was washed with saturated brine and dried over magnesium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (hexane/ethyl acetate) to obtain the title compound (1.72 g, 31%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09440922B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-1515b36c859648d1a5dd4503c6364978 |
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| 出典メモ | uspto-grants-2016_09 |
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