関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Fluoro-3-(trifluoromethyl)phenol | HCID 2737586 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 2-Fluoro-1-methoxy-3-(trifluoromethyl)benzene | HCID 2774768 | 91% |
反応手順
A mixture of 2-fluoro-3-(trifluoromethyl)-phenol (4.87 g, 27.04 mmol) and iodomethane (4.60 g, 32.4 mmol) in acetone (50 mL) is cooled to 0° C. and then 325 mesh potassium carbonate (4.48 g, 32.4 mmol) is added. The reaction is warmed to rt and stirred for 17 hours under N2. The reaction filtered to remove the solids, and the filtrate is acidified with 1 N HCl. The mixture is diluted with water and extracted with Et2O. The organic layer is dried (Na2SO4), and the solvent is removed in vacuo to afford 4.76 g (91%) of 2-fluoro-3-methoxybenzotrifluoride that is utilized without purification. Rf=0.35 (4/1 hexanes/EtOAc). 1H NMR (400 MHz, CDCl3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07608639B2 |
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| 出典データセット | uspto-grants-2009_10 |
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| ORD ID | ord-c8bf09d1edef465493d84ff7d9649785 |
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| 出典メモ | uspto-grants-2009_10 |
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