참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | 2-Methoxycarbonyl-3-methyl-4-nitrobenzenesulfonyl chloride | HCID 15334533 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-Methyl-5-nitrosaccharin | HCID 15334534 | — |
반응 단계
104 ml of 25% 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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05723415 |
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| 출처 데이터셋 | uspto-grants-1998_03 |
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| ORD ID | ord-9750ebabdd9f4e72aa5a98408ce4247f |
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| 출처 메모 | uspto-grants-1998_03 |
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