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 | HCID 68575380 | HCID 68575380 | — |
| 反応物 | 1-[4-(2,3-Difluorophenyl)-1,3-thiazol-2-yl]piperazine | HCID 68776289 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 4-[4-(2,3-difluorophenyl)-1,3-thiazol-2-yl]-N-pyridin-3-ylpiperazine-1-carboxamide | HCID 11589426 | 55% |
反応手順
A mixture of 2,2,2-trichloroethyl pyridin-3-ylcarbamate (211 mg, 0.782 mmol), 1-[4-(2,3-difluorophenyl)-1,3-thiazol-2-yl]piperazine (200 mg, 0.711 mmol) and diisopropylethylamine (0.248 ml, 1.42 mmol) in dimethyl sulfoxide (2.5 ml) was stirred at 70° C. for 15 hours. Water was poured to 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 give 157 mg (55.0%) of the desired product as a solid. mp 172-173° C.
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-cb1c431329fe4aba86706b1fb07ddfe3 |
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| 出典メモ | uspto-grants-2010_12 |
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