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Methanesulfonyl chloride → 2-Chloro-4-fluorophenyl methanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | 2-Chloro-4-fluorophenol | HCID 74814 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 2-Chloro-4-fluorophenyl methanesulfonate | HCID 9837431 | 92.3% |
反応手順
To a mixture of 2-chloro-4-fluorophenol (14.7 g) and methylsulfonyl chloride (11.5 g), under ice-cooling, pyridine (30 g) was added dropwise. The resulting mixture was stirred at room temperature for 30 minutes to complete the methylsulfonylation, after which the pyridine was distilled off under reduced pressure. Toluene and water were added to the residue and the mixture was washed with a dilute aqueous hydrochloric acid, then with water. The toluene layer as separated was dried over anhydrous sodium sulfate and then the toluene was distilled off to afford the titled compound (20.8 g) as a pale yellow oil. After purification by silica gel chromatography, the oil was made colorless with a refractive index nD23 =1.5117.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04752326 |
| 出典データセット | uspto-grants-1988_06 |
| ORD ID | ord-6fa1ac8d2b4b4539bfc9f3fb4b48d7c2 |
| 出典メモ | uspto-grants-1988_06 |