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Potassium Carbonate → 2-((3,5-dimethylisoxazol-4-yl)methyl)-2H-tetrazol-5-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Aminotetrazole | HCID 20467 | — |
| 反応物 | Isoxazole, 4-(chloromethyl)-3,5-dimethyl- | HCID 88246 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-((3,5-dimethylisoxazol-4-yl)methyl)-2H-tetrazol-5-amine | HCID 57422459 | 40% |
反応手順
2H-tetrazol-5-amine (1.29 g, 12.5 mmol), 4-(chloromethyl)-3,5-dimethylisoxazole (1.56 mL, 12.5 mmol) and potassium carbonate (1.73 g, 15.5 mmol) in DMF (20 mL) were heated to 80° C. with stirring for 16 hours. The reaction was cooled to room temperature, diluted with dichloromethane (100 mL) and washed consecutively with brine and water. The organics were dried over sodium sulfate and concentrated with rotary evaporation. The crude product was purified by silica gel chromatography (0-10% gradient ethyl acetate/dichloromethane) affording 2-((3,5-dimethylisoxazol-4-yl)methyl)-2H-tetrazol-5-amine as a white crystalline solid (970 mg, 40% yield) MS M+H calculated 195.1, found 195.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08076491B2 |
| 出典データセット | uspto-grants-2011_12 |
| ORD ID | ord-b692dd97deb14fa1a55faf407fa54f84 |
| 出典メモ | uspto-grants-2011_12 |