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Water → 4-Chloro-2-fluoro-5-methoxybenzyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Chloromethyl Methyl Ether | HCID 7864 | — |
| 反応物 | 2-Chloro-4-fluoroanisole | HCID 2773580 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Titanium Tetrachloride | HCID 24193 | — |
| 生成物 | 4-Chloro-2-fluoro-5-methoxybenzyl chloride | HCID 18408344 | 68% |
反応手順
17.6 g (0.11 mol) of 2-chloro-4-fluoroanisole was dissolved in a dichloromethane solution of 1N titanium tetrachloride, and 88.3 g (1.10 mol) of methoxymethyl chloride was dropwise added thereto at room temperature, followed by stirring at room temperature for 5 hours. After completion of the reaction, the reaction solution was poured into water, followed by stirring at room temperature for 2 hours, and then the aqueous phase was removed The organic layer was dried over anhydrous magnesium sulfate, and the solvent was distilled off. Then, the obtained residue was purified by silica gel column chromatography to obtain 15.5 g (yield: 68%) of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06472348B1 |
| 出典データセット | uspto-grants-2002_10 |
| ORD ID | ord-4e75cf6b6849448486d1734f943a47e4 |
| 出典メモ | uspto-grants-2002_10 |