참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium Chloride | HCID 5234 | — |
| 반응물 | 1,3-Dimethyl 2-[2-nitro-4-(trifluoromethyl)phenyl]propanedioate | HCID 2763558 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | Methyl 2-(2-nitro-4-(trifluoromethyl)phenyl)acetate | HCID 83569 | — |
반응 단계
2-(2-Nitro-4-trifluoromethylphenyl)-malonic acid dimethyl ester (68 g, 0.21 mol) was dissolved in dimethyl sulfoxide (200 mL). Sodium chloride (34 g, 0.58 mol) and water (60 mL) were added and the mixture was stirred for 16-20 h at 120° C. (reaction monitored by TLC). The reaction mixture was then cooled to room temperature and quenched into water, which caused precipitation of the product. After stirring for 30 minutes, the product. (45 g, 80%) was isolated by filtration. The product was used without further purification in the next reaction. A small sample was crystallized (EtOAc/hexane, 2:8) for analysis, to yield yellow crystals, mp 104-105° C. 1H NMR (CDCl3) 8.3 (s, 1H), 7.88 (d, J=8.4 Hz, 1H), 7.50 (d, J=8.4 Hz, 1H), 4.12 (s, 2H), 3.60 (s, 3H). MS (FAB) m/z: 275.2 (M++1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08377958B2 |
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| 출처 데이터셋 | uspto-grants-2013_02 |
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| ORD ID | ord-980dbeea74934c869152bdc20e9429a5 |
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| 출처 메모 | uspto-grants-2013_02 |
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