関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | O-Xylene | HCID 7237 | — |
| 反応物 | 2,3-Dichloronitrobenzene | HCID 18555 | — |
| 反応物 | 4-Methylpentane-1,2-diol | HCID 91171 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 生成物 | 1-Chloro-2-fluoro-3-nitrobenzene | HCID 75016 | — |
反応手順
In a 1-liter flange flask fitted with a distillation bridge and stirrer, 29 g (0.06 mol) of polyethylene glycol dimethyl ether 500 and 139 g (2.4 mol) of potassium fluoride were introduced at 120° C. into the melt of 576 g (3.0 mol) of 2,3-dichloronitrobenzene. Subsequently, 20 g (0.19 mol) of xylene were added and the reaction suspension was azeotropically dried by application of a vacuum of 60 mbar and heating to 150° C. After the xylene had been distilled off, the distillation bridge was replaced by a reflux condenser, the reaction suspension was heated to 190° C. and stirred for 6 hours at this temperature. Amount of 3-chloro-2-fluoronitrobenzene formed: 11 GC area-% after 6 hours.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05476976 |
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| 出典データセット | uspto-grants-1995_12 |
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| ORD ID | ord-df61fe4428ee4cf3a2dcd11342b20919 |
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| 出典メモ | uspto-grants-1995_12 |
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