関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1-(4-Phenyl-1,3-thiazol-2-yl)piperazine | HCID 712468 | — |
| 反応物 | 2,2,2-Trichloroethyl[6-(acetylamino)pyridin-3-yl]carbamate | HCID 86245259 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | N-[6-(Acetylamino)pyridin-3-yl]-4-(4-phenyl-1,3-thiazol-2-yl)piperazine-1-carboxamide | HCID 68779653 | 13.7% |
反応手順
A mixture of 2,2,2-trichloroethyl [6-(acetylamino)pyridin-3-yl]carbamate (293 mg, 0.897 mmol), 1-(4-phenyl-1,3-thiazol-2-yl)piperazine (200 mg, 0.815 mmol) and diisopropylethylamine (0.156 ml, 0.897 mmol) in dimethylsulfoxide (2.7 ml) was stirred at 70° C. for 15 hours. Water was poured into the reaction mixture and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate) and recrystallized from a mixed solvent of hexane and tetrahydrofuran to obtain the desired product (47.3 mg, 13.7%) as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07851473B2 |
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| 出典データセット | uspto-grants-2010_12 |
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| ORD ID | ord-28ddafc44ba942d0ad509f83d5ab655e |
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| 出典メモ | uspto-grants-2010_12 |
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