関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Phenoxyacetamidine Hydrochloride | HCID 2745912 | — |
| 反応物 | 2-Bromo-1-[4-(4-fluorophenoxy)phenyl]propan-1-one | HCID 86012610 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-[4-(4-fluorophenoxy)phenyl]-5-methyl-2-(phenoxymethyl)-1H-imidazole | HCID 11406190 | — |
反応手順
620 mg of 2-phenoxyethanimidamide hydrochloride (0.00333 mol) are desalified in dichloromethane by the action of a 3N sodium hydroxide solution. After decantation and extraction of the aqueous phase by dichloromethane, the organic phase is dried over sodium sulphate then evaporated to dryness. The white powder obtained is solubilized in dimethylformamide (30 ml). 275 mg of 2-bromo-1-[4-(4-fluorophenoxy)phenyl]propan-1-one (0.000851 mol) is added. The mixture is heated at 50° C. for 20 hours then returned to 23° C. before adding 25 ml of water and 30 ml of ethyl acetate. After extraction with ethyl acetate, the organic phase is dried over sodium sulphate then evaporated in a rotary evaporator under vacuum. The residue obtained is adsorbed on silica then purified by chromatography on a Biotage-type silica column (eluent: ethyl acetate-heptane: 2-8). A pale yellow-coloured foam is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07534805B2 |
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| 出典データセット | uspto-grants-2009_05 |
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| ORD ID | ord-001b0d8372e0418badf9340602733873 |
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| 出典メモ | uspto-grants-2009_05 |
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