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Water → 1-(3-Chloro-2-methoxymethoxyphenyl)-1-(2-methoxyphenyl)ethanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Methoxy-1-phenylethanone | HCID 77698 | — |
| 反応物 | 1-Chloro-2-(methoxymethoxy)benzene | HCID 542624 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 1-(3-Chloro-2-methoxymethoxyphenyl)-1-(2-methoxyphenyl)ethanol | HCID 19812679 | — |
反応手順
1-Chloro-2-methoxymethoxybenzene (20.0 g) was combined with 72.5 ml of 1.6 M n-butyl lithium in hexane at 0° C. with stirring and allowed to react for 4 hours. A solution of 16.0 ml of 2-methoxyacetophenone in 20 ml of tetrahydrofuran was then added with stirring. After a short reaction period, water and ether were added and the ether layer was dried over magnesium sulfate, filtered, and concentrated by evaporation under reduced pressure to obtain an oil. This was purified by liquid chromatography, eluting with a 95:5 mixture of hexane and ethyl acetate, to obtain 6.67 g of the title compound as an oil. The assigned structure was consistent with the proton NMR spectrum.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04999448 |
| 出典データセット | uspto-grants-1991_03 |
| ORD ID | ord-20f35688785146699d63a7c3bac505d9 |
| 出典メモ | uspto-grants-1991_03 |