関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2,4-Dichloro-alpha-(chloromethyl)benzenemethanol | HCID 94351 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (+-)-alpha-(2,4-Dichlorophenyl)-1H-imidazole-1-ethanol | HCID 32238 | 66.3% |
反応手順
30 g of sodium were added to a solution of 88.5 g of imidazole in 600 ml of methanol; the solvent was then evaporated off. The residue was dissolved in 300 ml of dimethylformamide and heated to 115°-120° C. To the solution so obtained was added, dropwise and under stirring, a solution of 225 g of 1-(2',4'-dichlorophenyl)-2-chloro-ethanol in 400 ml of dimethylformamide. The mixture was heated to 115°-120° C. and maintained at that temperature for 20 minutes and, after subsequent cooling to 40° C., 2500 ml of iced water were added under vigorous stirring. The product precipitated under stirring over a period of about two hours, the upper liquid was then decanted off, a further 2500 ml of water were added and, after standing, the whole was filtered. The precipitate thus obtained was dried and crystallized from toluene. 170 g of the desired product, melting at 134°-135° C., was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04221803 |
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| 出典データセット | uspto-grants-1980_09 |
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| ORD ID | ord-f5e27aea74774ac9bd2760a0a0f55d0f |
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| 出典メモ | uspto-grants-1980_09 |
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