関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-(Chloromethyl)-1-methylbenzimidazole | HCID 248044 | — |
| 反応物 | 2-Fluoro-4-hydroxy-5-methoxybenzaldehyde | HCID 598155 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 2-fluoro-5-methoxy-4-(1-methyl-1H-benzimidazol-2-ylmethoxy)-benzaldehyde | HCID 59803873 | 267.3% |
反応手順
To a solution of 2-fluoro-4-hydroxy-5-methoxy-benzaldehyde (39, 3.0 g, 5 mmol) in N,N-dimethylacetamide (120 mL) was added sodium hydride (60% dispersion in mineral oil, 0.8 g, 19 mmol) portion wise. After the addition was complete, the reaction was stirred for 30 minutes after which 2-chloromethyl-1-methyl-1H-benzoimidazole (212, 2.9 g, 16 mmol) was added and then heated at 80° C. overnight. The reaction mixture was then poured into water (1 L) with stirring and the precipitated solid was filtered, washed with water and dried to give the desired compound (213, 4.2 g, 84% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07872018B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-5745c0bd33554da4aea5d3f33ddc96d3 |
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| 出典メモ | uspto-grants-2011_01 |
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