참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Ethyl dichloroacetate | HCID 10808 | — |
| 반응물 | 1,3-Difluoro-5-nitrobenzene | HCID 75272 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Ethyl 2-chloro-2-(2,6-difluoro-4-nitrophenyl)ethanoate | HCID 21260294 | 97% |
반응 단계
A solution of 3,5-difluoronitrobenzene (20 g,126 mmol) and ethyl dichloroacetate (15.8 ml, 129 mmol) in DMF (60 ml) was added to potassium t-butoxide (31.8 g, 283 mmol) in DMF (500 ml) at −25° C. over 30 minutes. The mixture was stirred for 15 minutes at −25° C. then poured on to a mixture of ice (600 g) and 2M hydrochloric acid (500 ml). The aqueous mixture was extracted with ethyl acetate, the combined extracts were washed with water and sodium hydrogen carbonate solution and dried (MgSO4) and the solvent removed by evaporation to give ethyl 2-chloro-2-(2,6-difluoro-4-nitrophenyl)ethanoate (34 g, 97%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06184225B2 |
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| 출처 데이터셋 | uspto-grants-2001_02 |
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| ORD ID | ord-ece5942eccfd41b9b50ac2ce665ab347 |
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| 출처 메모 | uspto-grants-2001_02 |
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