참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | Ethane, 2-bromo-1,1-diethoxy- | HCID 74852 | — |
| 반응물 | 2,3-Difluoro-4-(2-hydroxyethyl)phenol | HCID 53416145 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-(4-(2,2-Diethoxyethoxy)-2,3-difluorophenyl)ethanol | HCID 57988989 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08148373B2 |
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| 출처 데이터셋 | uspto-grants-2012_04 |
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| ORD ID | ord-495f26dc0f6d400596f1373aca5a746f |
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| 출처 메모 | uspto-grants-2012_04 |
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