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Acetic Acid → 2-Fluoro-5-methoxybenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | Oxygen | HCID 977 | — |
| 反応物 | 4-Fluoro-3-methylanisole | HCID 137546 | — |
| 触媒 | Cobalt(II) acetate tetrahydrate | HCID 61372 | — |
| 生成物 | 2-Fluoro-5-methoxybenzoic acid | HCID 2774543 | — |
反応手順
The title compound was prepared according to a method reported by Hay and Blanchard [Canad. J. Chem. 43, 1306 (1965)]. In a three-necked round-bottom flask (1000 mL), equipped with a magnetic stirrer, thermometer, reflux condensor and a gas distribution tube, cobalt(II)acetate tetrahydrate (12.6 g; 51 mmol) was dissolved in glacial acetic acid (404 mL) by stirring. Commercial 4-fluoro-3-methylanisole (35.4, 252 mmol) and 33% HBr in acetic acid (10.1 mL; 51 mmol) were added and then the mixture was heated on an oil-bath to 90°-95° C. All the time a stream of oxygen was passed through the solution at a rate of about 660 mL/min. After 3 hours the reaction mixture was cooled to room temperature and then rotary evaporated to dryness.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05420151 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-40ae4c13385b4ac8936fb6c2114f24a0 |
| 出典メモ | uspto-grants-1995_05 |