関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Methoxyphenol | HCID 9007 | — |
| 反応物 | tert-Butyl methyl ether | HCID 15413 | — |
| 触媒 | Zirconium chloride (ZrCl4), (T-4)- | HCID 9856075 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Tert-butyl-3-methoxyphenol | HCID 12252976 | 20% |
反応手順
To a suspension of zirconium tetrachloride (2.3 g, 10 mmol) in methylene dichloride (30 ml) was added methyl tert-butyl ether (0.88 g, 10 mmol) at 0° C. After stirring at 0° C. for 30 minutes, 3-methoxyphenol (1.24 g, 10 mmol) in methylene dichloride was added and the mixture was stirred for 2 hours at ambient temperature. The reaction was quenched with saturated aqueous sodium bicarbonate, followed by the addition of methylene dichloride. Then, the organic layer was separated, dried over magnesium sulfate, filtered off, evaporated under reduced pressure to give a residue, which was applied to a silica gel chromatography column eluted with a volume mixture of hexane and ethylacetate (20/1 to 4/1) to furnish 360 mg (20% yield) of the title compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07214824B2 |
|---|
| 出典データセット | uspto-grants-2007_05 |
|---|
| ORD ID | ord-aee84e76d0484b708a5c56fffb3a1794 |
|---|
| 出典メモ | uspto-grants-2007_05 |
|---|