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Potassium Carbonate → 4-nitro-2-(1H-1,2,4-triazol-1-yl)pyridine 1-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Chloro-4-nitropyridine 1-oxide | HCID 84433 | — |
| 反応物 | 1-Trimethylsilyl-1,2,4-triazole | HCID 87558 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-nitro-2-(1H-1,2,4-triazol-1-yl)pyridine 1-oxide | HCID 66721386 | 27.2% |
反応手順
To a solution of 2-chloro-4-nitropyridine 1-oxide (2.00 g, 11.4 mmol) and 1-(trimethylsilyl)-1H-1,2,4-triazole (1.64 mL, 11.4 mmol) in DMF (40 mL), was added potassium carbonate (4.75 g, 34.4 mmol). The reaction mixture was allowed to stir at rt for 2 h. The DMF was evaporated and water was added. The precipitate was filtered and washed with water then hexane and dried under vacuum. The solid was purified by column to give 4-nitro-2-(1H-1,2,4-triazol-1-yl)pyridine 1-oxide (0.643 g, 27.1%) as a pale yellow solid. LCMS: (FA) ES+ 208.1, ES− 206.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08110687B2 |
| 出典データセット | uspto-grants-2012_02 |
| ORD ID | ord-f5ff02d794014095bf81206b1d4540ab |
| 出典メモ | uspto-grants-2012_02 |