참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Nitrate | HCID 24434 | — |
| 반응물 | 3-(Trifluoromethoxy)benzoic acid | HCID 66096 | — |
| 용매 | Sulfuric Acid | HCID 1118 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2-Nitro-5-(trifluoromethoxy)benzoic acid | HCID 21904613 | — |
반응 단계
To a solution of 3-trifluoromethoxybenzoic acid (49.0 g, 0.24 mol) in sulfuric acid (500 mL) at less than 0° C. (ice-MeOH bath) was added a solution of potassium nitrate (31.3 g, 0.31 mol) in sulfuric acid (200 mL) over 20 minutes. The resulting solution was stirred at 0° C. for 2 hours, then warmed to room temperature and stirred for 18 hours. The reaction was poured into ice and the resulting acidic solution was extracted with EtOAc (5×). The combined organics were washed with H2O (1×), brine (2×), H2O (1×) and brine (1×), dried (Na2SO4), filtered and concentrated in vacuo to give the crude sub-title compound (65.7 g) as a solid contaminated with HOAc. The crude sub-title compound was dissolved in EtOAc and toluene and concentrated in vacuo to give a HOAc free solid (58.4 g, 97%) that was used in the next step without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07129233B2 |
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| 출처 데이터셋 | uspto-grants-2006_10 |
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| ORD ID | ord-2d151f92b9ff41c58507c2ca4bb34a54 |
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| 출처 메모 | uspto-grants-2006_10 |
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