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聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 2-(Acetylamino)-2-[[3-methoxy-2-(phenylmethoxy)phenyl]methyl]-propanedioic acid, diethyl ester
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 反应物 | 乙酰氨基丙二酸二乙酯 | HCID 14041 | — |
| 反应物 | 乙醇钠 | HCID 2723922 | — |
| 反应物 | 3-(Chloromethyl)-2-phenylmethoxyanisole | HCID 22402454 | — |
| 溶剂 | 醋酸 | HCID 176 | — |
| 溶剂 | 乙醇 | HCID 702 | — |
| 产物 | 2-(Acetylamino)-2-[[3-methoxy-2-(phenylmethoxy)phenyl]methyl]-propanedioic acid, diethyl ester | HCID 131718168 | 66.4% |
反应步骤
A quantity of 136.20 g (0.42 mole) of 21 wt.% sodium ethoxide in ethanol is added to a stirred solution of 90.14 g (0.415 mole) of diethyl acetamidomalonate (Aldrich) in 800 mL of absolute ethanol. A solution of the benzyl chloride derivative of Example 38 in 500 mL of absolute ethanol is added and the mixture is heated at reflux for 2 hours. The cooled mixture is poured into 4 L of ice and water containing 20.0 g of glacial acetic acid. The supernatant is decanted from the separated gum. The gum is dissolved in 2 L of ether, the solution dried (magnesium sulfate), and concentrated to ca 300 mL volume. Petroleum ether (100 mL) is added to precipitate 107.1 g (66.4% yield) of pure crystalline product; mp 94°-96° C.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US05246943 |
| 来源数据集 | uspto-grants-1993_09 |
| ORD ID | ord-f93f0562c268458cb7f1687b9cb17055 |
| 来源说明 | uspto-grants-1993_09 |