関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2',4'-Dihydroxyacetophenone | HCID 6990 | — |
| 反応物 | 1-Bromooctane | HCID 8140 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(2-Hydroxy-4-octyloxy-phenyl)-ethanone | HCID 10468007 | — |
反応手順
A slurry of 2,4-dihydroxy actophenone (3.8 g; 25 mmol) and KHCO3 (2.75 g; 27.5 mmol) in DMF (50 mL) was stirred at 50° C. for 1 hour and then added 1-bromooctane (4.75 mL; 27.5 mmol). The reaction mixture was stirred at 50-60° C. for 7 days, poured onto H2O (100 mL) and the aqueous phase extracted with diethyl ether (3×). The combined organic fractions was dried (MgSO4), filtered, evaporated to dryness and purified by column chromatography (SiO2; EtOAc/PE80-100° C.=1:10) to yield 4.39 g (66%) as yellow oil. MS (direct; Cl): 265 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741352B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-608f69a0b7be4c06a95c0fdcf4ccd517 |
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| 出典メモ | uspto-grants-2010_06 |
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