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海萝胶 → 2-(4-(1-Hydroxyethyl)phenyl)-5-decyloxypyrimidine
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 海萝胶 | HCID 313 | — |
| 反应物 | (5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 | HCID 887 | — |
| 反应物 | 二甲基对苯二胺二盐酸 | HCID 14798 | — |
| 反应物 | (-)-(4-(1-Acetoxy-ethyl)phenyl)-5-decyloxypyrimidine | HCID 19694897 | — |
| 溶剂 | 甲苯 | HCID 1140 | — |
| 溶剂 | 四氢呋喃 | HCID 8028 | — |
| 产物 | 2-(4-(1-Hydroxyethyl)phenyl)-5-decyloxypyrimidine | HCID 21468280 | 98.5% |
反应步骤
Into 100 ml of methanol and 50 ml of tetrahydrofuran were dissolved 15 g of the (-)-2-{4-(1-acetoxyethyl)phenyl}-5-decyloxypyrimidine obtained in Preparation Example [starting material compound (VI)] 70, and then 50 ml of 20% aqueous sodium hydroxide solution were added thereto, to subject to reaction at 40° to 45° C. for 4 hours. After completion of the reaction, 4N hydrochloric acid was added to the reaction mixture to adjust it to pH 7 to 8, and then 200 ml of toluene were added to effect extraction and separation. After the organic phase was washed with water, the solvent was distilled off under reduced pressure to obtain 13.2 g (yield: 98.5%) of (-)-2-{4-(1-hydroxyethyl)phenyl}-5-decyloxypyrimidine.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US05389293 |
| 来源数据集 | uspto-grants-1995_02 |
| ORD ID | ord-4a53a7e9919e42328dec9c7a8d87cefc |
| 来源说明 | uspto-grants-1995_02 |