化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 6-Bromo-3-chloro-2-fluorobenzotrifluoride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 反応物 | 4-Bromo-2-fluoro-3-(trifluoromethyl)aniline | HCID 53669714 | — |
| 触媒 | Cuprous chloride | HCID 62652 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 6-Bromo-3-chloro-2-fluorobenzotrifluoride | HCID 53632443 | — |
反応手順
A solution of sodium nitrite (7.3 g) in concentrated sulphuric acid was added to a stirred cooled solution of 4-bromo-2-fluoro-3-trifluoromethylaniline (27.4 g) in glacial acetic acid while maintaining the temperature below 15° C. The mixture was stirred at 10°-15° C. for one and a half hours then poured into a mixture of copper (I) chloride (10.5 g) in hydrochloric acid (5M). The mixture was stirred for one and a half hours then diluted with water, extracted with ether, washed with aqueous sodium hydroxide solution (2M), water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness and the residue was distilled to give 6-bromo-3-chloro-2-fluorobenzotrifluoride (8.3 g) as a yellow oil b.p. 44°-45° C./2 mbar.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05856274 |
| 出典データセット | uspto-grants-1999_01 |
| ORD ID | ord-fdf4db2069834267a19313abb8d6b659 |
| 出典メモ | uspto-grants-1999_01 |