関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrofluoric Acid | HCID 14917 | — |
| 反応物 | Antimony pentachloride | HCID 24294 | — |
| 反応物 | 1-Chloro-4-(1,1-dichloro-2,2,2-trifluoroethoxy)benzene | HCID 13691059 | — |
| 生成物 | 4-(1-Chloro-1,2,2,2-tetrafluoroethoxy)chlorobenzene | HCID 20151895 | 89.8% |
反応手順
A 500 ml polytetrafluoroethylene reactor equipped with stirrer, thermometer and reflux condenser is charged with 55.9 g (0.2 mol) of 4-(1,1-dichloro-2,2,2-trifluoroethoxy)chlorobenzene in 100 ml of hydrogen fluoride. 3.0 g (0.01 mol; corresponding to 5 mol%) of antimony pentachloride are added at a temperature in the range from -5° C. to 0° C. The resultant hydrogen chloride is removed from the reactor through the reflux condenser. After 20 minutes at 0° C., the evolution of hydrogen chloride ceases. Excess hydrogen fluoride is removed by distillation, the residue is dissolved in 200 ml of methylene chloride and the solution is extracted with water. The organic phase is separated by distillation, affording 47.3 g (89.8% of theory) of 4-(1-chloro-1,2,2,2-tetrafluoroethoxy)chlorobenzene. Boiling point 181° C., nD25 =1.4362.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04727187 |
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| 出典データセット | uspto-grants-1988_02 |
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| ORD ID | ord-30de9da655d044c9895a8b402380e49a |
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| 出典メモ | uspto-grants-1988_02 |
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