関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Methoxycarbonyl-3-methyl-4-nitrobenzenesulfonyl chloride | HCID 15334533 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Methyl-5-nitrosaccharin | HCID 15334534 | — |
反応手順
104 ml of 25 percent ammonia solution are initially taken, 100 ml of water are added and a solution of 48.7 g (0.166 mol) of 2-methoxycarbonyl-3-methyl-4-nitrobenzenesulfonyl chloride in 70 ml of tetrahydrofuran is then added dropwise at 10° C. After stirring at 25° C. for three hours, water and THF are removed by concentration on a rotary evaporator, and the residue which remains is stirred with ethyl acetate, filtered off with suction and washed with ethyl acetate. After drying under reduced pressure, 34 g (0.131 mol)=79% of theory of a white solid of m.p.: 312° C. (dec.) are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05716905 |
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| 出典データセット | uspto-grants-1998_02 |
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| ORD ID | ord-e14a33f1974548acb39583963fe8fb9b |
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| 出典メモ | uspto-grants-1998_02 |
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