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3,4-Dimethoxybenzophenone → Methyl 3-(3,4-Dimethoxyphenyl)-3-phenylacrylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3,4-Dimethoxybenzophenone | HCID 286742 | — |
| 反応物 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 反応物 | Methyl 3,3-bis-(3,4-dimethoxyphenyl)acrylate | HCID 9820154 | — |
| 反応物 | Trimethylphosphonoacetate | HCID 53413272 | — |
| 生成物 | Methyl 3-(3,4-Dimethoxyphenyl)-3-phenylacrylate | HCID 54371031 | — |
反応手順
Methyl 3-(3,4-Dimethoxyphenyl)-3-phenylacrylate was prepared analogously to methyl 3,3-bis-(3,4-dimethoxyphenyl)acrylate using 3,4-dimethoxybenzophenone (4.8 g, 20 mmol), trimethylphosphonoacetate (4.1 g, 22 mmol) and lithium hexamethyldisilazide (22 mL, 22 mmol, 1 M) with a reaction time of 138 hours at reflux. The crude mixture was purified by flash column chromatography (silica gel, 1% ethyl acetate/methylene chloride) to afford 14.39 g (73%) of a mixture of the E and Z isomers as an oil. The isomers were separated by additional purification (silica gel, 1% ethyl acetate/methylene chloride) to afford pure samples of each of the isomers.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05929117 |
| 出典データセット | uspto-grants-1999_07 |
| ORD ID | ord-83eb26e9272c43958eb32cb66b52f3ac |
| 出典メモ | uspto-grants-1999_07 |