関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 15-Crown-5 | HCID 36336 | — |
| 反応物 | Methyl (2-bromo-5-methoxyphenyl)acetate | HCID 10658910 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-(2-Bromo-5-methoxy-phenyl)-2-ethyl-butyric acid | HCID 66835356 | — |
反応手順
(2-Bromo-5-methoxy-phenyl)-acetic acid methyl ester (3.51 g, 13.5 mmol) was dissolved in DMF (4.5 ml), and added with NaH (2.1 g, 67.7 mmol). Subsequently, 15-crown-5 (1.38 ml, 6.8 mmol) and EtI (5.5 ml, 67.7 mmol) cooled to 0° C. were added to the mixture. The mixture was diluted with ethyl acetate and washed with water and saturated brine. The residues obtained after concentration under reduced pressure were purified by silica gel column (hexane-ethyl acetate). Then, the resultant was dissolved in ethanol (80 ml) and water (80 ml), added with KOH (91 g), and stirred at 140° C. The reaction solution was extracted with ethyl acetate, and washed with water and saturated brine. After concentration under reduced pressure, the target compound was obtained (10.62 g, 78%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09126931B2 |
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| 出典データセット | uspto-grants-2015_09 |
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| ORD ID | ord-515fd476b674485e96f072808d02c3a4 |
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| 出典メモ | uspto-grants-2015_09 |
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