関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 3,4-Diethoxycarbonyl-5-nitro-6-phenyl-2-(p-tolylsulfonyl)pyridine | HCID 19935608 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 15289703 | HCID 15289703 | 43.8% |
反応手順
In 10 ml of ethanol was suspended 0.35 g of 3,4-diethoxycarbonyl-5-nitro-6-phenyl-2-(p-tolylsulfonyl)pyridine, whereto 2 ml of acetic acid and 0.15 g of reduced iron were added. The mixture was stirred at 80° C. for 4.5 hours. After ethanol was distilled off, the residue was neutralized with an aqueous solution of sodium hydrogencarbonate, followed by extraction with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried over sodium sulfate, followed by concentration under reduced pressure. The residue was subjected to silica gel flash column chromatography with chloroform/ethyl acetate (4:1) as the eluent, to give 0.144 g of the title compound.
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-d81733510f8c40759ff6e0729b255bef |
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| 出典メモ | uspto-grants-1995_05 |
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