関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Diethyl 2-hydroxy-5-nitro-6-phenylpyridine-3,4-dicarboxylate | HCID 19935597 | — |
| 生成物 | 2-Chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine | HCID 19935587 | — |
反応手順
In 6.5 ml of phosphorus oxychloride was dissolved 2.5 g of 3,4-diethoxycarbonyl-5-nitro-6-phenyl-2pyridone, followed by addition of 1 ml of DMF. The mixture was heated at 100° C. for 30 minutes. After the reaction mixture was concentrated under reduced pressure, an aqueous solution of sodium hydrogencarbonate was added to the residue for neutralization, followed by extraction with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. After the solvent was distilled off, the residue was subjected to silica gel column chromatography (eluent:ethyl acetate/hexane 1:2), to give 1.9 g of the title compound as yellow needles.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05420275 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-e1042bcf07c04ef68cc62404a8ba4b14 |
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| 出典メモ | uspto-grants-1995_05 |
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