関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | alpha-Phenyl[1,1'-biphenyl]-4-methanol | HCID 95512 | — |
| 反応物 | Thionyldiimidazole | HCID 21946057 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Bifonazole | HCID 2378 | — |
反応手順
13.6 g (0.2 mol) of imidazole are dissolved in 150 ml of acetonitrile and 3.5 ml of thionyl chloride are added at 10° C. 13 g (0.05 mol) of (biphenyl-4-yl)-phenyl-carbinol are added to the solution of thionyl-bis-imidazole thus obtained. After standing for 15 hours at room temperature, the solvent is removed by distillation in vacuo. The residue is taken up in chloroform and the solution is washed with water. The organic phase is collected, dried over sodium sulfate and filtered and the solvent is distiller off in vacuo. The oily residue is dissolved in ethyl acetate and freed from insoluble, resinous constituents by filtration. The solvent is again distilled off in vacuo and the residue is purified by recrystallization from acetonitrile. 8.7 g (56% of theory) of (biphenyl-4-yl)-imidazol-1-yl-phenylmethane [alternatively named as diphenyl-imidazolyl-(1)-phenyl-methane or as 1-(α-biphenyl-4-ylbenzyl)imidazole] of melting point 142° C. are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04118487 |
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| 出典データセット | uspto-grants-1978_10 |
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| ORD ID | ord-9b15d528063b40abb29e802c515022ea |
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| 出典メモ | uspto-grants-1978_10 |
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