関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1H-imidazole-2-carbaldehyde | HCID 24955 | — |
| 反応物 | 2-Bromoethyl ethyl ether | HCID 61141 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(2-ethoxyethyl)-1H-imidazole-2-carbaldehyde | HCID 59408708 | 17% |
反応手順
To a solution of imidazole-2-carboxaldehyde (2.00 g, 21 mmol) in DMF (1 mL) was added 1.1 eq. of 1-bromo-2-ethoxyethane (3.51 g, 22 mmol), potassium carbonate and a catalytic amount of potassium iodide. The reactions were heated at 110° C. for 18 hrs followed by evaporation to dryness and purified utilizing a Biotage SP4 with a gradient method of 5-50% methanol in DCM to yield the desired compound (580 mg, 3.56 mmol, 17% yield). 1H NMR (400 MHz, DMSO-d6) δ 9.63 (s, H), 7.6 (s, H), 7.21 (s, H), 4.45 (dd, 2H), 3.62 (dd, 2H), 3.38 (m, 2H), 1.05 (t, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08840865B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-cf435f512b2f4463971637ac5ed95ded |
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| 出典メモ | uspto-grants-2014_09 |
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