関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 6-(2,4-Dichlorophenyl)-5-(4-chlorophenyl)-2-oxo-1,2-dihydropyridine-3-carbonitrile | HCID 21984825 | — |
| 生成物 | 2-Chloro-5-(4-chlorophenyl)-6-(2,4-dichlorophenyl)nicotinonitrile | HCID 10150677 | — |
反応手順
To 6-(2,4-Dichlorophenyl)-5-(4-chlorophenyl)-2-oxo-1,2-dihydropyridine-3-nitrile (40.75g) was added POCl3 (20 mL). The reaction was heated to 100° C. for 13 hours. After cooling to room temperature the excess POCl3 was removed in vacuo before the residue was dissolved in CH2Cl2 and washed with saturated aqueous NaHCO3 solution. The solution was concentrated and purified via flash chromatography on silica gel with a gradient elution of 30% to 100% CH2Cl2 in hexane affording the title compound. HPLC/MS: 392.9 (M+1), 394.9 (M+3); Rt=4.45 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728141B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-f6e58b0c76784b2495f47166236c83c3 |
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| 出典メモ | uspto-grants-2010_06 |
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