関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Hexyl p-Toluenesulfonate | HCID 220448 | — |
| 反応物 | 2-(4-(1-Hydroxyethyl)phenyl)-5-decyloxypyrimidine | HCID 21468280 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (+)-2-{4-(1-Hexyloxyethyl)phenyl}-5-decyloxypyrimidine | HCID 54404658 | 82.1% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05389293 |
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| 出典データセット | uspto-grants-1995_02 |
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| ORD ID | ord-b893edb234c34782b8663ea06395fd3f |
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| 出典メモ | uspto-grants-1995_02 |
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