参与物
| 角色 | 名称 | HCID | 投料 |
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| 反应物 | 氢化钠 | HCID 24758 | — |
| 反应物 | 2-氰基苯甲酸 | HCID 220448 | — |
| 反应物 | 2-(4-(1-Hydroxyethyl)phenyl)-5-decyloxypyrimidine | HCID 21468280 | — |
| 溶剂 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 产物 | (+)-2-{4-(1-Hexyloxyethyl)phenyl}-5-decyloxypyrimidine | HCID 54404658 | 82.1% |
反应步骤
Into 20 ml of anhydrous dlmethylformamide were dissolved 1.78 g (5 millimole) of the (+)-2-{4-(1-hydroxyethyl)phenyl}-5-decyloxypyrimidine obtained in Preparation Example [starting material compound (VI)] 70, and then 0.24 g (6 millimole) of 60% sodium hydride was added thereto, followed by stirring at 40° C. for 1 hour. Subsequently, 1.79 g (7 millimole) of hexyl p-toluenesulfonate were added thereto, to subject to reaction at the same temperature for 2 hours. After completion of the reaction, the reaction mixture was poured into 200 ml of water, extracted with 200 ml of toluene, followed by separation thereof, and the organic phase was washed with water sufficiently, followed by drying over anhydrous magnesium sulfate. After the solvent was distilled off under reduced pressure, the resulting residue was purified by silica gel column chromatography (eluent; toluene: ethyl acetate) to obtain 1.81 g (yield: 82%) of (+)-2-{4-(1-hexyloxyethyl)phenyl}-5-decyloxypyrimidine.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US05389293 |
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| 来源数据集 | uspto-grants-1995_02 |
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| ORD ID | ord-b893edb234c34782b8663ea06395fd3f |
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| 来源说明 | uspto-grants-1995_02 |
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