関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethyl dichloroacetate | HCID 10808 | — |
| 反応物 | 1,3-Difluoro-5-nitrobenzene | HCID 75272 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl 2-chloro-2-(2,6-difluoro-4-nitrophenyl)ethanoate | HCID 21260294 | 97% |
反応手順
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%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06184225B2 |
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| 出典データセット | uspto-grants-2001_02 |
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| ORD ID | ord-ece5942eccfd41b9b50ac2ce665ab347 |
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| 出典メモ | uspto-grants-2001_02 |
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