関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 4-Pyrrolidinopyridine | HCID 75567 | — |
| 反応物 | 4-(Decyloxy)benzoic acid | HCID 138527 | — |
| 反応物 | (+)-4-[3-{2(S)-methylbutoxy}propyl]phenol | HCID 22844682 | — |
| 生成物 | (+)-4-[3-{2(S)-methylbutoxy}propyl]phenyl 4-decyloxybenzoate | HCID 22844683 | 90.4% |
反応手順
Into a four-necked flask equipped with a stirrer and a thermometer were charged 1.11 g (5 millimole) of (+)-4-[3-{2(S)-methylbutoxy}propyl]phenol, 1.67 g (6 millimole) of 4-decyloxybenzoic acid and 30 ml of anhydrous dichlomethane, and then 1.22 g (6 millimole) of N,N'-dicyclohexylcarbodiimide and 0.1 g of 4-pyrrolidinopyridine were added thereto, followed by stirring at room temperature for one day. After completion of the reaction, precipitates formed were filtered off and diluted with 200 ml of toluene. The organic phase was washed with water, 5% aqueous acetic acid solution, water, 5% aqueous sodium hydrogen carbonate solution and water in this order and then dried over anhydrous magnesium sulfate, followed by concentration under reduced pressure. The obtained residue was purified by silica gel column chromttography (eluent: toluene-ethyl acetate) to obtain 2.18 g (yield: 90.4%) of (+)-4-[3-{2(S)-methylbutoxy}propyl]phenyl 4-decyloxybenzoate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05264151 |
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| 出典データセット | uspto-grants-1993_11 |
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| ORD ID | ord-808005c4d12d4f4fa01d6268e9eeae2f |
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| 出典メモ | uspto-grants-1993_11 |
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