関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Benzenesulfonyl chloride | HCID 7369 | — |
| 反応物 | 2,5-Difluoroaniline | HCID 67775 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-(2,5-difluorophenyl)benzenesulfonamide | HCID 8500589 | — |
反応手順
0.194 mole (25 g) of 2,5-difluoroaniline is added to 125 ml of pyridine. 0.2 mole (25.5 ml) of benzenesulphonyl chloride is added, while the temperature is between 35° C. and 45° C. The temperature is maintained at 40° C. for 1 hour after the addition is completed, and then the reaction mixture is poured onto 1 kg of ice and water to which 100 ml of concentrated hydrochloric acid have been added. The expected product precipitates. After filtration and washing, it is treated with a normal sodium hydroxide solution in order to remove insoluble material. The soda-containing filtrate is neutralized with concentrated hydrochloric acid. The expected product, which has precipitated, is filtered off, washed to neutrality and recrystallized from acetic acid. It melts at 115° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04725283 |
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| 出典データセット | uspto-grants-1988_02 |
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| ORD ID | ord-3dbdfcae709944628a41bf0158fca242 |
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| 出典メモ | uspto-grants-1988_02 |
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