関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | 1-Chloro-2,4-dimethylbenzene | HCID 523153 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(2,4-Dimethylphenyl)-1H-imidazole | HCID 10130177 | 48% |
反応手順
30 mmol of 2,4-dimethylchlorobenzene (4.2 g), 40 mmol of imidazole (2.7 g), 35 mmol of NaOEt solution in ethanol (10% by weight) and 230 mg of trans-di-μ-chlorobis[2-[bis(1,1-dimethylethyl)phosphino]-2-methylpropyl-C,P]dipalladium(II) (1.0 mol %) are suspended in 50 ml of THF and heated at 110° C. in a pressure tube for 9 hours. After removal of the salts by filtration, the solvent is removed under reduced pressure. This gives crude 1-(2,4-dimethylphenyl)imidazole as a brown liquid which can be purified by distillation (boiling point: 122° C./12 torr); yield: 48%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06353136B1 |
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| 出典データセット | uspto-grants-2002_03 |
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| ORD ID | ord-5b8e81b3e9e441b5918ccc6788957777 |
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| 出典メモ | uspto-grants-2002_03 |
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