関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Nitrourea | HCID 62372 | — |
| 反応物 | 4-(2,3,4,5,6-Pentafluorophenoxy)piperidine | HCID 14837040 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-Aminocarbonyl-4-(2,3,4,5,6-pentafluorophenoxy)piperidine | HCID 19762462 | 73.4% |
反応手順
A solution of 4.0 g of 4-(2,3,4,5,6-pentafluorophenoxy)piperidine in 100 ml of 95% ethanol was treated with 1.73 g of nitrourea and then stirred at 65° C. for five hours. After cooling to room temperature, the reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with water followed by a saturated sodium chloride solution and dried over anhydrous magnesium sulfate. Filtration, followed by evaporation of the solvents afforded a residue which was purified by means of high pressure liquid chromatography (silica gel; elution with 5% methanol/dichloromethane). The resultant solid was recrystallized from hot isopropanol to yield 3.41 g (73.3%) of 1-aminocarbonyl-4-(2,3,4,5,6-pentafluorophenoxy)piperidine, m.p. 170°-172° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05212184 |
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| 出典データセット | uspto-grants-1993_05 |
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| ORD ID | ord-9d6390a6c1ee4c4f86c013f205aa450a |
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| 出典メモ | uspto-grants-1993_05 |
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