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, the mixture is concentrated on a rotary evaporator to remove water and THF. 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 | US05716906 |
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| 出典データセット | uspto-grants-1998_02 |
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| ORD ID | ord-395d1e72089a49fbb95a04ac0a1739c6 |
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| 出典メモ | uspto-grants-1998_02 |
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