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2',4',6'-Trihydroxyacetophenone → 1-[2,4,6-Trihydroxy-3,5-di(3-methyl-2-buten-1-yl)phenyl]ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2',4',6'-Trihydroxyacetophenone | HCID 68073 | — |
| 反応物 | 4-Bromo-2-methylbut-1-ene | HCID 549585 | — |
| 溶媒 | Potassium Hydroxide | HCID 14797 | — |
| 生成物 | 1-[2,4,6-Trihydroxy-3,5-di(3-methyl-2-buten-1-yl)phenyl]ethanone | HCID 10979627 | 38.7% |
反応手順
1-(2,4,6-trihydroxyphenyl]ethanone (2.0 mg, 11.9 mmol) was dissolved in a 5% potassium hydroxide aqueous solution (20 mL). After the mixture was cooled below 0° C., isopentenyl bromide (3.6 g, 24 mmol) was slowly added dropwise within 30 min. The reaction mixture was stirred at room temperature for 2 hours, then poured into an ice water and acidified to pH 2. The reaction mixture was extracted with ethyl acetate. The extract was collected and dried over anhydrous sodium sulfate. After removal of the solvent, the residue was purified by silica gel column chromatography (dichloromethane as eluent) to give the desired compound (0.7 g, yield 20%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09090583B2 |
| 出典データセット | uspto-grants-2015_07 |
| ORD ID | ord-3cb7b15b61034ec69b25282892b2f98a |
| 出典メモ | uspto-grants-2015_07 |