化工社化工社 化学情報印刷レポート · 研究参考用
Pyridine → 4-Bromo-4'-isopropyloxybiphenyl
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 1,4-Dibromobenzene | HCID 7804 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Isopropoxyphenol | HCID 82001 | — |
| 触媒 | Copper oxide (CuO) | HCID 164827 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Bromo-4'-isopropyloxybiphenyl | HCID 20087281 | 49.5% |
反応手順
To a mixture of Example 1A (505 mg, 3.31 mmol), 1,4-dibromobenzene (2.34 g, 9.92 mmol.), K2CO3 (960 mg, 6.87 mmol) and pyridine (20 mL) at 80° C. was added Cu(II) oxide (650 mg, 8.17 mmol). After the addition, the mixture was refluxed vigorously for 20 h. After cooling, methylene chloride was added and the mixture was filtered through Celite. The filtrate was concentrated to dryness. The residue was dissolved in ether, which was washed with 10% HCl (2×), 1N NaOH (2×), brine (1×), dried over MgSO4, and concentrated to dryness. The residue was purified on silica gel eluting with hexane and ethyl acetate gradient to give the desired product as a white solid (477 mg, 47%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07928243B2 |
| 出典データセット | uspto-grants-2011_04 |
| ORD ID | ord-d3ec91c6c2514aac86d7966d1b7523e5 |
| 出典メモ | uspto-grants-2011_04 |