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Sodium Sulfite → 3,4-Diethoxycarbonyl-5-nitro-6-phenyl-2-sulfopyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 反応物 | 2-Chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine | HCID 19935587 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3,4-Diethoxycarbonyl-5-nitro-6-phenyl-2-sulfopyridine | HCID 19935609 | 59.9% |
反応手順
A solution of 0.28 g of sodium sulfite in 7 ml of water was added to a solution of 0.70 g of 2-chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine in 7 ml of ethanol, and the mixture was heated under reflux for minutes. After the reaction mixture was concentrated, the concentrate was acidified with 1N HCl, followed by extraction with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over magnesium sulfate. After concentration to dryness under reduced pressure, the residue was recrystallized from chloroform/ether, to give 0.47 g of white crystals.
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-b90069235e134fd59f7501c27c3f1a71 |
| 出典メモ | uspto-grants-1995_05 |