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Sodium hydride → HCID 69740515、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1,4-Dichloro-cis-2-butene | HCID 6432115 | — |
| 反応物 | N-butyl-N-(1H-benzoimidazol-2-ylmethyl)-2,3-difluorobenzamide | HCID 22394018 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | HCID 69740515 | HCID 69740515 | — |
反応手順
N-butyl-N-(1H-benzoimidazol-2-ylmethyl)-2,3-difluorobenzamide (226 mg, 0.66 mmol) was dissolved in 3 mL dimethylacetamide at room temperature. Sodium hydride (29 mg, 0.72 mmol, 60% oil dispersion) was added and the reaction mixture stirred 5 minutes. Cis-1,4-Dichloro-2-butene was added and the reaction mixture stirred 90 minutes. The reaction mixture was diluted with 10 mL ethyl acetate, placed in a separatory funnel and washed 1×10 mL H2O then 1×10 mL brine. The organic phase was dried over MgSO4, filtered, concentrated, then purified by flash chromatography eluting with 1/1 ethyl acetate/hexane to afford 206 mg 2,3-difluoro-N-butyl-N-[(4-chlorobut-2-enyl)-1H-benzoimidazol-2-ylmethyl]-benzamide.
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-dec45ae1438d4949a46841b7dc461363 |
| 出典メモ | uspto-grants-2005_06 |