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-Bromo-1,1-dimethoxyethane | HCID 81672 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(2,2-dimethoxyethyl)-1H-imidazole-2-carbaldehyde | HCID 28284458 | 32% |
反応手順
To a solution of the imidazole-2-carboxaldehyde (0.41 g, 4.27 mmol) in DMF (1 mL) was added 1.1 eq. of 2-bromo-1,1-dimethoxyethane (0.79 g, 4.69 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 (248 mg, 1.35 mmol, 32% yield). 1H NMR (400 MHz, DMSO-d6) δ 9.9 (s, H), 7.85 (s, H), 7.55 (s, H), 5.82 (m, H), 4.75 (d, 2H), 3.45 (s, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09433594B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-51437833e8544546b140e98642bce904 |
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| 出典メモ | uspto-grants-2016_09 |
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