関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Ethyl 4-(bromomethyl)benzoate | HCID 954261 | — |
| 反応物 | 5,6-Dichloro-2-(2,2,2-trifluoro-ethyl)-1H-indole | HCID 66968833 | — |
| 反応物 | dichloro-2-(2,2,2-trifluoro-ethyl)-1H-benzoimidazole | HCID 66968977 | — |
| 生成物 | 1-(2-Bromo-benzyl)-5,6-dichloro-2-(2,2,2-trifluoro-ethyl)-1H-benzoimidazole | HCID 44430139 | — |
反応手順
NaH (60%) 120 mg, 3 mmol) was added into a solution of dichloro-2-(2,2,2-trifluoro-ethyl)-1H-benzoimidazole. 5,6-Dichloro-2-(2,2,2-trifluoro-ethyl)-1H-indole (538 mg, 2 mmol) in DMF (5 ml) at 0° C. The resulting mixture was stirred at 0° C. for half hour. Ethyl 4-(bromomethyl)-benzoate (729.3 mg, 3 mmol) and potassium iodide (498 mg, 3 mmol) were then added to the reaction mixture at 0° C. The reaction temperature was raised to 25° C. and then the reaction mixture was stirred for 18 hours. NH4Cl (aq.) was added and extracted with EtOAc. The organic layer was washed with brine, then dried over anhydrous MgSO4. The solvent was distilled out under reduced pressure. Column chromatography (silica gel, EtOAc/hexanes (0% to 60%) yielded the title compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07566733B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-2416a624f1ad42318eada988864f5255 |
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| 出典メモ | uspto-grants-2009_07 |
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