関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 3-Pentanol | HCID 11428 | — |
| 反応物 | 5-[((Phenylsulfonyl)amino)carbonyl]-pyridine-2-carboxylate | HCID 19928173 | — |
| 触媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | HCID 54318896 | HCID 54318896 | — |
反応手順
5 drops of concentrated sulfuric acid were added to 0.9 g (2.94 mmol) of 5-[((phenylsulfonyl)amino)carbonyl]-pyridine-2-carboxylate in 30 ml of 3-pentanol, while stirring, and the mixture was heated at 90° C. for 6 hours. The excess 3-pentanol was distilled off in vacuo and the residue was treated with ethyl acetate. The crystalline crude product was combined with the product obtained from the mother liquor by purification by column chromatography (melting point 186° to 187° C.), treated with hot ethyl acetate, cooled, filtered off with suction and washed with ethyl acetate. This gave 0.55 g of the colorless title compound, melting point 182° to 183° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05428046 |
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| 出典データセット | uspto-grants-1995_06 |
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| ORD ID | ord-6bd2cbbffc724748a70641fce04391fe |
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| 出典メモ | uspto-grants-1995_06 |
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