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Water → 5,6-difluoro-1H-1,3-benzodiazol-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cyanogen Bromide | HCID 10476 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1,2-Diamino-4,5-difluorobenzene | HCID 2736755 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 5,6-difluoro-1H-1,3-benzodiazol-2-amine | HCID 10678708 | 40% |
反応手順
4,5-Difluorobenzene-1,2-diamine (0.651 g, 0.562 mmol, commercially available from Matrix Scientific) in acetonitrile (10 mL) and water (2 ml) at 0° C. was treated with cyanogen bromide (0.063 g, 0.6 mmol). The reaction mixture was allowed to warm to room temperature, and then stirred for 14 hours. The reaction mixture was then treated with saturated aqueous sodium hydrogen carbonate solution (50 ml) and shaken. The resulting solid was filtered off, washed with water and dried under reduced pressure to give 0.39 g of 5,6-difluoro-1H-benzo[d]imidazol-2-amine (yield, 40%). MS (EI): 186 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08088767B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-d0e0bd4bbee149338404daac09d120bf |
| 出典メモ | uspto-grants-2012_01 |