関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 3-Fluoroaniline | HCID 9742 | — |
| 反応物 | 1H-Indazole-5-sulfonyl chloride | HCID 22567144 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | N-(3-fluorophenyl)-(1H-indazol-5-yl)sulfonamide | HCID 10266270 | — |
反応手順
N-(3-Fluorophenyl)-(1H-indazol-5-yl)sulfonamide can be obtained in the following way: 0.98 ml of 3-fluoroaniline is added dropwise to a solution, cooled to a temperature in the region of 0° C., of 2.57 g of (1H-indazol-5-yl)sulfonyl chloride in 40 ml of pyridine. Stirring is maintained for 2 hours at a temperature in the region of 0° C. and then for 18 hours at a temperature in the region of 20° C. The medium is concentrated by evaporation under reduced pressure, and the residue obtained is taken up with 50 ml of ethyl acetate and 40 ml of water. The organic phase is washed with 2 times 20 ml of water, dried over magnesium sulfate, filtered and concentrated by evaporation under reduced pressure. The residue obtained is purified by chromatography on a silica column with an ethyl acetate/cyclohexane (1/3 by volume) mixture as eluent. 8 mg of N-(3-fluorophenyl)-(1H-indazol-5-yl)sulfonamide are thus obtained in the form of an orange solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06858638B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-7aef0a420cdb497b899c709993003b79 |
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| 出典メモ | uspto-grants-2005_02 |
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