関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dichloro-4-nitrobenzene | HCID 7443 | — |
| 反応物 | Stearyltrimethylammonium chloride | HCID 8155 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 生成物 | 1,2-Dichloro-4-nitrobenzene | HCID 7443 | 13.6% |
| 生成物 | 2-Chloro-1-fluoro-4-nitrobenzene | HCID 67688 | 90.6% |
反応手順
70 g (0.2 mol) of octadecyltrimethylammonium chloride were dissolved in a melt of 2020 g (10.5 mol) of 3,4-dichloronitrobenzene at 50° C. with stirring, 580 g (10.0 mol) of potassium fluoride were suspended at 100° C. and this suspension was heated to 180° C. for 9 h. After cooling to about 60° C., the reaction suspension was filtered with suction, the liquid adhering to the residue was distilled off at 150° C./70 torr and the combined organic phases were fractionated with the addition of an auxiliary base as an acid scavenger. 1445 g (90.6%, relative to 3,4-dichloronitrobenzene converted) of 3-chloro-4-fluoronitrobenzene and 324 g (13.6%, relative to 3,4-dichioronitrobenzene employed) of unreacted 3,4-dichloronitrobenzene were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05545768 |
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| 出典データセット | uspto-grants-1996_08 |
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| ORD ID | ord-75a60b16d1cf4861ae8b4f00980cd542 |
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| 出典メモ | uspto-grants-1996_08 |
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