참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Lauric Acid | HCID 3893 | — |
| 반응물 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 반응물 | 4-Pyrrolidinopyridine | HCID 75567 | — |
| 반응물 | 2-(4-(1-Hydroxyethyl)phenyl)-5-decyloxypyrimidine | HCID 21468280 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | (+)-2-{4-(1-Dodecanoyloxyethyl)phenyl}-5-decyloxypyrimidine | HCID 21468295 | 94% |
반응 단계
Into 20 ml of dichloromethane were dissolved 1.78 g (5 millimoles) of the (+)-2-{4-(1-hydroxyethyl)phenyl}-5-decyloxypyrimidine obtained in Preparation Example [starting material compound (VI)]70 and 1.2 g (6 millimoles) of dodecanic acid, and then 1.4 g of N,N'-dicyclohexylcarbodiimide and 0.1 g of 4-pyrrolidinopyridine were added thereto, followed by stirring at room temperature for 24 hours. After completion of the reaction, the precipitates were filtered off and 200 ml of toluene were added thereto, followed by washing with water, 5% acetic acid, water, 5% aqueous sodium hydrogen carbonate solution and water in this order. After the organic phase was dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent; toluene:ethyl acetate) to obtain 2.53 g (yield: 94%) of (+)-2-{4-(1-dodecanoyloxyethyl)phenyl}-5-decyloxypyrimidine. The physical values are shown in Table-1.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05389293 |
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| 출처 데이터셋 | uspto-grants-1995_02 |
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| ORD ID | ord-2026f0e84e994620be221f3c645de7d2 |
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| 출처 메모 | uspto-grants-1995_02 |
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