関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 2-Chlorophenol | HCID 7245 | — |
| 反応物 | Ethyl bromoacetate | HCID 7748 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl 2-(2-chlorophenoxy)acetate | HCID 302826 | 97.6% |
反応手順
To a solution of 2-chlorophenol (2.06 mL, 19.9 mmol) in DMF (40 mL) is added potassium carbonate (3.03 g, 21.9 mmol) and ethyl bromoacetate (2.3 mL, 20.7 mmol), and the mixture is stirred at 80° C. for 18 h. Et2O is added, and the mixture is washed with water, brine, dried (MgSO4), and filtered. The filtrate is evaporated, and the residue is purified by chromatography in silica gel; elution with EtOAc:dichloromethane:hexane (10:5:85) gives 4.17 g of the product 465. 1H NMR (CDCl3) δ 7.38 (d, 1H), 7.21 (t, 1H), 6.92 (t, 1H), 6.84 (d, 1H), 4.70 (s, 2H), 4.27 (q, 2H), 1.29 (t, 3H); MS: m/z 215, 217 (M++1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07741493B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-b29967885a46478f8ec56bcdaffb4281 |
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| 出典メモ | uspto-grants-2010_06 |
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