関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,4-Bis(4-methoxyphenyl)-6-chloropyridazine | HCID 12568084 | — |
| 反応物 | Water methylene chloride | HCID 21908982 | — |
| 反応物 | HCID 178418255 | HCID 178418255 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 3,4-Bis(4-methoxyphenyl)-6-phenylpyridazine | HCID 12113842 | 36.9% |
反応手順
3,4-Bis(4-methoxyphenyl)-6-chloropyridazine [Eur. J. Med. Chem.-Chimica Therapeutica, 14, 53-60 (1979)] (309.3 mg, 0.95 mmol) was dissolved in benzene (2 ml). Tetrakis(triphenylphosphine)palladium [Pd(Ph3P)4] (90.6 mg, 0.08 mmol) and phenylmagnesium bromide (1.0 M tetrahydrofuran solution) (1.5 ml) were then added successively, followed by stirring at 60° C. for 75 minutes. After water-methylene chloride was added to the reaction mixture, the mixture was extracted with methylene chloride and the organic layer was dried over anhydrous sodium sulfate. The solvent was distilled off and the residue was then separated and purified by chromatography on a silica gel column [silica gel (40 g), hexane/ethyl acetate (2/1)], whereby the title compound was obtained as a pale yellow amorphous solid (129 mg, 36.9%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06664256B1 |
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| 出典データセット | uspto-grants-2003_12 |
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| ORD ID | ord-b3638a0bd3904b26a3442cfa33b7aabb |
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| 出典メモ | uspto-grants-2003_12 |
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