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Benzyl Alcohol → HCID 11735856、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzyl Alcohol | HCID 244 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 2-Methyl-4-pentenoyl chloride | HCID 12921442 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 11735856 | HCID 11735856 | 78.3% |
反応手順
To a 0° C. solution of 23.8 g of benzyl alcohol, 0.05 g of 4-(dimethylamino)pyridine, 18.3 g of pyridine and 250 ml of methylene chloride is added, dropwise, a solution of 29.5 g of racemic 2-methyl-4-pentenoyl chloride in 50 ml of methylene chloride. The mixture is stirred at room temperature for 4 hours, followed by successive washing with 2N hydrochloric acid, saturated sodium bicarbonate and saturated sodium chloride. The organic layer is dried and concentrated in vacuo. The residue is purified by Kugelrohr distillation to give 35.2 g of the desired product as a colorless oil; bp 70°-75° C. at 0.10 mm Hg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05356885 |
| 出典データセット | uspto-grants-1994_10 |
| ORD ID | ord-e034fe3030ad4579aa1c167f3273b062 |
| 出典メモ | uspto-grants-1994_10 |