関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 6-Hydrazinylpyridine-3-sulfonamide | HCID 12096590 | — |
| 反応物 | N-(1-ethoxy-ethylidene)-4-methyl-benzamide | HCID 21894679 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 6-(3-Methyl-5-p-toly-[1,2,4]triazole-1-yl)-pyridine-3-sulfonic acid amide | HCID 10215232 | 54% |
反応手順
N-(1-ethoxy-ethylidene)-4-methyl-benzamide 429 mg (2.09 mmol) was dissolved in a mixed solvent of dichloromethane 20 ml and methanol 10 ml, and 6-hydrazinopyridine-3-sulfonic acid amide 433 mg (2.23 mmol) was added to the solution 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, 6-(3-methyl-5-p-toly-[1,2,4]triazole-1-yl)-pyridine-3-sulfonic acid amide (372 mg, yield: 54%) 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 | US07135572B2 |
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| 出典データセット | uspto-grants-2006_11 |
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| ORD ID | ord-83e39186048c4451829669b8ce650a6d |
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| 出典メモ | uspto-grants-2006_11 |
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