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Potassium Fluoride → 2-Chloro-4,5-difluorobenzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 反応物 | 2,4-Dichloro-5-fluorobenzonitrile | HCID 2782753 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 2-Chloro-4,5-difluorobenzonitrile | HCID 4085849 | 68.6% |
反応手順
A mixture comprising 5.70 g (0.03 mol) of 2,4-dichloro-5-fluorobenzonitrile, 3.48 g (0.06 mol) of spray dried KF and 30 ml of dimethylsulfoxide, was reacted at a temperature of from 140° to 150° C. for 3.5 hours in a glass reactor. After completion of the reaction, the mixture was poured into ice water (50 ml) and extracted with chloroform. The chloroform extract was washed five times with water and then dried. Then chloroform was distilled off. The residue was distilled under reduced pressure to obtain 3.57 g (yield: 68.6%) of 2-chloro-4,5-difluorobenzonitrile. Boiling point: 105°-107° C./37 mmHg; melting point: 35°-37° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05332851 |
| 出典データセット | uspto-grants-1994_07 |
| ORD ID | ord-6bc9dc00baca4272a4c1fb4f5e1ef79e |
| 出典メモ | uspto-grants-1994_07 |