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-(4-Fluorophenyl)-2-thiazolyl]piperazine | HCID 8027201 | — |
| 反応物 | HCID 86245257 | HCID 86245257 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | N-(3,4-Dimethylisoxazol-5-yl)-4-[4-(4-fluorophenyl)-1,3-thiazol-2-yl]piperazine-1-carboxamide | HCID 68776294 | 50.2% |
反応手順
A mixture of 2,2,2-trichloroethyl (3,4-dimethylisoxazol-5-yl)carbamate (240 mg, 0.834 mmol), 1-[4-(4-fluorophenyl)-1,3-thiazol-2-yl]piperazine (200 mg, 0.760 mmol) and diisopropylethylamine (0.265 ml, 1.52 mmol) in dimethylsulfoxide (2.5 ml) was stirred at 70° C. for 18 hours. Water was poured into the reaction solution, 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 recrystallized from a mixed solvent of hexane and tetrahydrofuran to give the desired product (153 mg, 50.2%) 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-15f35b7610864667b01816b72ddcb72f |
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| 出典メモ | uspto-grants-2010_12 |
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