참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 4-Cyanobenzenesulfonyl chloride | HCID 39497 | — |
| 반응물 | Benzenamine, 4-chloro-N-ethyl-2-nitro- | HCID 97006 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4'-Chloro-4-cyano-N-ethyl-2'-nitrobenzenesulfonanilide | HCID 18509265 | 64.6% |
반응 단계
To a suspension of sodium hydride (60%, 0.10 g (2.50 mmol)) in tetrahydrofuran (THF)(3.0 ml), 4-chloro-N-ethyl-2-nitroaniline (0.40 g (1.99 mmol)) was added with stirring at room temperature. To the mixture, after stirring for 30 minutes at room temperature, 4-cyanobenzenesulfonyl chloride (0.50 g (2.48 mmol)) was added and the resulting mixture was stirred at room temperature for 3 hours. The reaction mixture was poured into water and the resulting mixture was extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography with ethyl acetate-hexane (1:2) as eluent, to give 0.47 g (64%) of the title compound as pale yellow crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06586617B1 |
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| 출처 데이터셋 | uspto-grants-2003_07 |
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| ORD ID | ord-ee92ba0fa7e3409690faf65a571f39f1 |
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| 출처 메모 | uspto-grants-2003_07 |
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