関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-Butanesulfonyl chloride | HCID 75430 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2,4-difluoro-N-(pyridin-3-ylmethyl)aniline | HCID 11096129 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(2,4-difluorophenyl)-N-(pyridin-3-ylmethyl)butanesulfonamide | HCID 14720307 | — |
反応手順
A 4.4 g. portion of 3-(2,4-difluorophenylaminomethyl)pyridine was dissolved in 15 ml. of dichloromethane, and to it were added 4.1 g. of potassium carbonate and 4.7 g. of butanesulfonyl chloride. The mixture was stirred under gentle reflux for several days, and was then cooled and diluted with 20 ml. of aqueous sodium bicarbonate and 5 ml. of aqueous sodium hydroxide. Some additional dichloromethane was added, and the suspension was shaken and the organic layer separated. It was washed with aqueous sodium bicarbonate and dried over magnesium sulfate, and it was then evaporated to a smaller volume and was chromatographed on a silica gel column, eluting with dichloromethane. The chromatography was repeated twice to obtain 0.38 g. of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04874775 |
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| 出典データセット | uspto-grants-1989_10 |
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| ORD ID | ord-9d3472ff94bf4e0a83f430fb815d192a |
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| 出典メモ | uspto-grants-1989_10 |
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