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 1,2,3-thiadiazol-5-ylcarbamate | HCID 68776945 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 4-(4-Phenyl-1,3-thiazol-2-yl)-N-1,2,3-thiadiazol-5-ylpiperazine-1-carboxamide | HCID 68776941 | 68.4% |
反応手順
A mixture of 2,2,2-trichloroethyl 1,2,3-thiadiazol-5-ylcarbamate (190 mg, 0.686 mmol), 1-(4-phenyl-1,3-thiazol-2-yl)piperazine (153 mg, 0.624 mmol) and diisopropylethylamine (0.217 ml, 1.25 mmol) in dimethyl sulfoxide (2.5 ml) was stirred at 70° C. for 3 days. 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 recrystallized from a mixed solvent of hexane and tetrahydrofuran to give 159 mg (68.4%) of the desired product 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-3b3a5f746c2d4e37a1e9ea3c9caedd91 |
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| 出典メモ | uspto-grants-2010_12 |
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