関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Hydrazinylbenzenesulfonamide hydrochloride | HCID 2794567 | — |
| 反応物 | Ethyl (1E)-N-benzoylethanimidate | HCID 13028604 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(3-Methyl-5-phenyl-[1,2,4]triazole-1-yl)-benzenesulfonamide | HCID 10193242 | 56% |
反応手順
N-(1-ethoxy-ethylidene)-benzamide 400 mg (2.09 mmol) was dissolved in a mixed solvent of dichloromethane 20 ml and methanol 10 ml and 4-hydrazinobenzenesulfonamide hydrochloride 515 mg (2.23 mmol) was added to the solution. Then, triethylamine 0.35 ml (2.51 mmol) was slowly added dropwise at room temperature for 10 minutes and stirred for 8 hours. After completing the reaction, water 20 ml was added to the reacting solution and extracted two times with dichloromethane, and then, the collected organic layer was washed with saturated brine. The organic layer was dried with anhydrous magnesium sulfate, filtered and concentrated under reduced pressure, and the resulting product was re-crystallized in acetone and hexane phase. As a result, 4-(3-methyl-5-phenyl-[1,2,4]triazole-1-yl)-benzenesulfonamide (368 mg, yield: 56%) was obtained as a solid phase.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07169929B2 |
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| 出典データセット | uspto-grants-2007_01 |
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| ORD ID | ord-0e704d54186e41ee9f02815bbcb12b3c |
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| 出典メモ | uspto-grants-2007_01 |
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