関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Ethane, 2-bromo-1,1-diethoxy- | HCID 74852 | — |
| 反応物 | 2,3-Difluoro-4-(2-hydroxyethyl)phenol | HCID 53416145 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(4-(2,2-Diethoxyethoxy)-2,3-difluorophenyl)ethanol | HCID 57988989 | — |
反応手順
Cesium carbonate (0.99 g) was added to a solution of 2,3-difluoro-4-(2-hydroxyethyl)phenol (example 77, step b) (0.44 g) and 2-bromo-1,1-diethoxyethane (0.4 mL) in DMF (10 mL). The resulting suspension was heated at 90° C. for 18 h. The reaction was allowed to cool and poured into water (100 mL). The aqueous mixture was extracted with diethylether (3×100 mL). The combined organic solutions were washed with water (200 mL) and brine (200 mL), dried over magnesium sulfate, filtered and evaporated. The crude material was purified by silica gel chromatography eluting with isohexane to 1:1 ethyl acetate:isohexane gradient. The fractions containing product were combined and evaporated to give the subtitled compound as a yellow oil. Yield 0.49 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08148373B2 |
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| 出典データセット | uspto-grants-2012_04 |
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| ORD ID | ord-495f26dc0f6d400596f1373aca5a746f |
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| 出典メモ | uspto-grants-2012_04 |
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