関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 6-Chloro-3-phenyl-4-(4-trifluoromethyl-phenyl)-pyridazine | HCID 21865189 | — |
| 反応物 | 7-Hydroxyquinoline | HCID 135426866 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 7-[6-Phenyl-5-(4-trifluoromethyl-phenyl)-pyridazin-3-yloxy]-quinoline | HCID 21865064 | — |
反応手順
To a solution of 6-chloro-3-phenyl-4-(4-trifluoromethyl-phenyl)-pyridazine, (Example 13 (e)), (106 mg, 0.3 mmol) and 7-hydroxyquinoline (55 mg, 0.4 mmol, Acros) in DMF (2.5 mL) was added NaH (22 mg, 0.6 mmol, 60% suspension in mineral oil, Aldrich) and the mixture was stired at room temperature for 15 h. The reaction mixture was then heated at 50° C. for another 28 h, allowed to cool to room temperature and the solvent removed in vacuum. The residue was partitioned between EtOAc/H2O and the aqueous layer was extracted with EtOAc. The combined organic layers were evaporated onto SiO2 and purified by flash silica gel chromatography with EtOAc/hexanes (0:1→3:7) as eluant to give the title compound as an off-white amorphous solid. Mp: 178–183° C. MS (ESI, pos ion.) m/z: 444 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07148221B2 |
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| 出典データセット | uspto-grants-2006_12 |
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| ORD ID | ord-18e33c20dad14892995dc3ff3fa0f3c5 |
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| 出典メモ | uspto-grants-2006_12 |
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