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3-Phenylprop-2-En-1-Ol → (3-Phenyl-2-propene-1-yl) 4,4-dimethoxy-3-oxobutyrate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Phenylprop-2-En-1-Ol | HCID 308 | — |
| 反応物 | Phosphate | HCID 1061 | — |
| 反応物 | Ethyl 4,4-dimethoxy-3-oxobutanoate | HCID 248327 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | (3-Phenyl-2-propene-1-yl) 4,4-dimethoxy-3-oxobutyrate | HCID 53702825 | — |
反応手順
2.68 g (14.1 mmol) of ethyl 4,4-dimethoxy-3-oxobutyrate, 5.14 ml (40.0 mmol) of cinnamyl alcohol and 244 mg (2.0 mmol) of 4-dimethylaminopyridine were heated under reflux in 40 ml of toluene for two nights. A phosphate buffer solution was added to the reaction liquid. After the extraction with ethyl acetate, the organic layer was washed with a saturated aqueous salt solution and then dried over anhydrous sodium sulfate. The solvent was distilled under reduced pressure, and the residue was purified by the silica gel chromatography (hexane/ethyl acetate=9/1) to obtain the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06995179B2 |
| 出典データセット | uspto-grants-2006_02 |
| ORD ID | ord-129c43881bba449a97daf6ee863e90ff |
| 出典メモ | uspto-grants-2006_02 |