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Benzaldehyde → Methyl 3-Hydroxy-2-methylene-3-phenylpropionate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzaldehyde | HCID 240 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methyl Acrylate | HCID 7294 | — |
| 反応物 | Dabco | HCID 9237 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Methyl 3-Hydroxy-2-methylene-3-phenylpropionate | HCID 9942369 | — |
反応手順
A mixture of benzaldehyde (63.67 g; 600 mmol), methyl acrylate (60 ml; 667 mmol) and 1,4-diazabicyclo [2.2.2] octane (13.46 g; 120 mmol) is stirred at ambient temperature for 119 hours. To the reaction solution is added water (60 ml), 37% hydrochloric acid (60 ml) and ethyl acetate (120 ml), and then, the organic phase is extracted. The resulting organic phase is washed twice with saturated saline (60 ml), dried over anhydrous sodium sulfate and filtered, then concentrated under reduced pressure, to give a crude product of the title compound at a yield of 108.8 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06031121 |
| 出典データセット | uspto-grants-2000_02 |
| ORD ID | ord-3cb3d5c663e44fe8a5662d593968671b |
| 出典メモ | uspto-grants-2000_02 |