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O-Xylene → 2,4-Dichloro-5-fluorobenzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | O-Xylene | HCID 7237 | — |
| 反応物 | 4-Methylpentane-1,2-diol | HCID 91171 | — |
| 反応物 | 1-Bromo-2,4-dichloro-5-fluorobenzene | HCID 11791393 | — |
| 反応物 | HCID 178418546 | HCID 178418546 | — |
| 触媒 | Tetrabutylphosphonium bromide | HCID 76564 | — |
| 生成物 | 2,4-Dichloro-5-fluorobenzonitrile | HCID 2782753 | — |
反応手順
97.6 g (0.4 mol) of 5-bromo-2,4-dichlorofluorobenzene, 35.8 g (0.4 mol) of copper(I)cyanide, 10.0 g (0.014 mol) of trimethyl(ethoxypolyoxypropyl)ammonium chloride, 5.0 g (0.015 mol) of tetrabutylphosphonium bromide and 5.0 g (0.01 mol) of polyethylene glycol dimethyl ether 500 were introduced together with 20.0 g (0.19 mol) of xylene into a 250 ml 3-neck flask fitted with a reflux condenser and blade stirrer and azeotropically dried at up to 150° C. under reduced pressure. Amount of 2,4-dichloro-5-fluorobenzonitrile formed: after 5 hours: 19 GC area-%. after 26 hours: 75 GC area-%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05492875 |
| 出典データセット | uspto-grants-1996_02 |
| ORD ID | ord-831c3ffd12e640e58d374f798b199218 |
| 出典メモ | uspto-grants-1996_02 |