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Sodium Bicarbonate → N-butyl-N-(1H-benzoimidazol-2-ylmethyl)-2,3-difluorobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2,3-Difluorobenzoyl chloride | HCID 519549 | — |
| 反応物 | 2-Butylaminomethylbenzimidazole | HCID 13169408 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-butyl-N-(1H-benzoimidazol-2-ylmethyl)-2,3-difluorobenzamide | HCID 22394018 | 58.2% |
反応手順
2-butylaminomethylbenzimidazole (2.6 g, 13 mmol) was dissolved in 30 mL toluene. Saturated NaHCO3 solution (30 mL) was added followed by 2,3-difluorobenzoyl chloride (1.3 mL, 10 mmol). The reaction mixture was stirred at room temperature for 3 hours. The reaction mixture was diluted with 100 mL ethyl acetate then washed 1×100 mL 1N NaOH followed by 1×100 mL H2O. The organic phase was dried over MgSO4, filtered, and then concentrated. The residue was purified by flash chromatography eluting with 1/1 ethyl acetate/hexane followed by ethyl acetate to afford 2.0 g N-butyl-N-(1H-benzoimidazol-2-ylmethyl)-2,3-difluorobenzamide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06906075B2 |
| 出典データセット | uspto-grants-2005_06 |
| ORD ID | ord-1c8f55698ef9426792c6276dac21d453 |
| 出典メモ | uspto-grants-2005_06 |