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Potassium Iodide → 2-Bromo-5-(2-ethoxyethoxy)-1,3-dimethylbenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethane, 1-chloro-2-ethoxy- | HCID 12341 | — |
| 反応物 | 4-Bromo-3,5-dimethylphenol | HCID 81970 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Bromo-5-(2-ethoxyethoxy)-1,3-dimethylbenzene | HCID 23157690 | 98% |
反応手順
To a solution of 4-bromo-3,5-dimethylphenol (12 g, 59.7 mmol), potassium iodide (1.5 g, 9.0 mmol) and potassium carbonate (9.9 g, 71.6 mmol) in N,N-dimethylformamide (80 mL) was added 2-chloroethyl ethyl ether (9.7 g, 89.3 mmol) at room temperature with stirring and the mixture was stirred at 70° C. for 2 days. The reaction mixture was cooled and concentrated under reduced pressure. The residue was partitioned between ethyl acetate and water. The organic layer was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=19/1) to give the title compound (15.9 g, yield 98%) as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07456218B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-d36509fef7d647219d495960856c54a5 |
| 出典メモ | uspto-grants-2008_11 |