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Imidazole → 1,4-Dichloro-2-(5-iodopent-1-ynyl)benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 5-(2,5-Dichlorophenyl)pent-4-yn-1-ol | HCID 22320759 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1,4-Dichloro-2-(5-iodopent-1-ynyl)benzene | HCID 12988942 | 72.5% |
反応手順
5-(2,5-Dichlorophenyl)pent-4-yn-1-ol (13.7 g, 59.8 mmol), triphenylphosphine (20.4 g, 77.8 mmol), and imidazole (5.71 g, 83.8 mmol) in a mixed solvent (100 ml acetonitrile-150 ml ether) was stirred under nitrogen at 0° C., and to this was slowly added iodine (21.3 g, 83.8 mmol). The solution was allowed to warm to room temperature and stirring was continued for 18 hours. This was chromatographed on silica gel with hexane to give the title compound (14.7 g, 72%), MS m/z 337.9 In the manner described in Example 30, above, the following alcohols in Table III were converted to the corresponding bromides:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06949661B2 |
| 出典データセット | uspto-grants-2005_09 |
| ORD ID | ord-388d448590f04dd8bd23169915047b87 |
| 出典メモ | uspto-grants-2005_09 |