関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Propionyl chloride | HCID 62324 | — |
| 反応物 | 2-(4-(1-Hydroxyethyl)phenyl)-5-decyloxypyrimidine | HCID 21468280 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (+)-2-(4-(1-Propanoyloxyethyl)phenyl}-5-decyloxypyrimidine | HCID 21468270 | 97% |
反応手順
Into 20 ml of pyridine were dissolved 1.78 g (5 millimole) of the (+)-2-{4-(1-hydroxyethyl)phenyl}-5-decyloxypyrimidine obtained in the Preparation Example starting material compound (VI)] 70, and then 0.56 g (6 millimole) of propionic chloride was added thereto, to subject to reaction at 30 to 40° C. for 2 hours. After completion of the reaction, the reaction mixture was poured into 200 ml of water, adjusted to pH 1 to 2 with 4N hydrochloric acid, and then extracted with 200 ml of toluene, followed by separation thereof. The organic phase was washed with water, 5% aqueous sodium hydrogen carbonate solution and water in this order. After drying over anhydrous magnesium sulfate, the residue obtained by distilling the organic solvent off under reduced pressure was purified by silica gel column chromatography (eluent; toluene: ethyl acetate) to obtain 2.00 g (yield: 97%) of (+)-2-(4-(1-Propanoyloxyethyl)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-b144768a10ff48e2938c7eaf39d68973 |
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| 出典メモ | uspto-grants-1995_02 |
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