참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Nitric Acid | HCID 944 | — |
| 반응물 | 3',5'-Bis(trifluoromethyl)acetanilide | HCID 723600 | — |
| 용매 | Sulfuric Acid | HCID 1118 | — |
| 생성물 | 1-Acetamido-2-nitro-3,5-bis(trifluoromethyl)benzene | HCID 19958574 | — |
반응 단계
To a solution of 1-acetamido-3,5-bis(trifluoromethyl)benzene (400 mg, 1.37 mmol) in concentrated H2SO4 (3 mL) at 0° C. was added dropwise 70% HNO3 (0.4 mL, Baker). The mixture was stirred at 0° C. for 0.5 h, then at room temperature for 3 h and it was poured into ice water (10 g). The precipitate was collected by filtration, affording 400 mg of crude product which contained two compounds by 1H NMR. It was separated on a column of silica gel, eluted with chloroform, to afford 134 mg of pure 1-acetamido-2-nitro-3,5-bis(trifluoromethyl)benzene as white long needles. mp: 190°-2° C., 1H NMR (CDCl3): δ 2.226 (s, 3H), 7.765 (s, 1H), 7.978 (s, 1H); 8.918 (s, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05620979 |
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| 출처 데이터셋 | uspto-grants-1997_04 |
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| ORD ID | ord-0efd3ef062964cf0acdd2fd1226f93bf |
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| 출처 메모 | uspto-grants-1997_04 |
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