関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1-Benzyl-1H-imidazole-5-carboxaldehyde | HCID 2773239 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 反応物 | 1-(3-Bromopropyl)-4-fluorobenzene | HCID 14737133 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-benzyl-5-(4-(4-fluorophenyl)-1-hydroxybutyl]-1H-imidazole | HCID 19421994 | 86% |
反応手順
5,4 g of magnesium turnings are covered with 50 ml of dry tetrahydrofuran. A solution of 1-bromo-3-(4-fluorophenyl)propane (48,7 g) in 200 ml of dry tetrahydrofuran is then added dropwise to the mixture at such a rate that a smooth reaction is maintained. After the addition is complete, the reaction mixture is refluxed for one additional hour and cooled to room temperature. To the reaction mixture is then added dropwise the solution of 1-benzyl-5-imidazolecarbaldehyde (20,9 g) in 200 ml of tetrahydrofuran. After the addition is complete, the reaction mixture is refluxed for 2 hours, cooled and poured into cold saturated ammonium chloride solution. Tetrahydrofuran phase is removed and the water phase is extracted three times with ethyl acetate. Organic phases are combined, dried and evaporated to dryness. The residue is suspended with diethyl ether and filtered. Yield 86%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05559141 |
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| 出典データセット | uspto-grants-1996_09 |
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| ORD ID | ord-ebc0367cb5794565b026ebd42a4a9b6f |
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| 出典メモ | uspto-grants-1996_09 |
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