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-(3-Phenyl-(1,2,4)thiadiazol-5-yl)-piperazine | HCID 2777760 | — |
| 反応物 | Bis(2,2,2-trichloroethyl) imidazo[1,2-b]pyridazin-6-ylimidodicarbonate | HCID 86625504 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | N-imidazo[1,2-b]pyridazin-6-yl-4-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine-1-carboxamide | HCID 68777839 | 85.7% |
反応手順
A mixture of bis(2,2,2-trichloroethyl) imidazo[1,2-b]pyridazin-6-ylimidodicarbonate (295 mg, 0.609 mmol), 1-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine (300 mg, 1.22 mmol) and diisopropylethylamine (0.106 ml, 0.609 mmol) in dimethylsulfoxide (2.0 ml) was stirred at 70° C. for 4 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 purified by silica gel column chromatography (ethyl acetate) and recrystallized from a mixed solvent of hexane and tetrahydrofuran to give 212 mg (85.7%) 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-67a8e63431db432dbc63bab2da1d51c0 |
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| 出典メモ | uspto-grants-2010_12 |
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