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4-Bromoanisole → 1-(4-methoxyphenyl)-1H-1,2,4-triazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Bromoanisole | HCID 7730 | — |
| 反応物 | 1H-1,2,4-Triazole | HCID 9257 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 触媒 | Cuprous chloride | HCID 62652 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(4-methoxyphenyl)-1H-1,2,4-triazole | HCID 11084390 | 44.5% |
反応手順
A mixture of 13.8 parts of 1H-1,2,4-triazole, 18.7 parts of 1-bromo-4-methoxybenzene, 5 parts of potassium carbonate, 0.5 parts of copper (I)chloride and 90 parts of N,N-dimethylformamide is stirred and refluxed for 2 days. The reaction mixture is cooled and poured onto water. The product is extracted twice with benzene. The combined extracts are washed with water, dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using trichloromethane as eluent. The pure fractions are collected and the eluent is evaporated. The residue is triturated in 2,2'-oxybispropane. The product is filtered off and dried, yielding 7.8 parts (44.5%) of 1-(4-methoxyphenyl)-1H-1,2,4-triazole; mp. 99.4° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04232034 |
| 出典データセット | uspto-grants-1980_11 |
| ORD ID | ord-d66f3bafed354632a5fbe55a039d4b7a |
| 出典メモ | uspto-grants-1980_11 |