関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phenylphosphonic dichloride | HCID 69990 | — |
| 反応物 | Diethyl 2-hydroxy-5-nitro-6-phenylpyridine-3,4-dicarboxylate | HCID 19935597 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine | HCID 19935587 | — |
反応手順
To 1.0 g of 3,4-diethoxycarbonyl-5-nitro-6-phenyl-2-pyridone was added 1.3 ml (3.37 eq.) of phenylphosphonic dichloride, and the mixture was heated at 150° C. for 2.5 hours. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride, and dried over magnesium sulfate. The solvent was distilled off, and the residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane 1:2), to give an oily product. Yield: 950 mg (90.5%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05420275 |
|---|
| 出典データセット | uspto-grants-1995_05 |
|---|
| ORD ID | ord-c122d6c730f541f4a3dcfbcfd6f66660 |
|---|
| 出典メモ | uspto-grants-1995_05 |
|---|