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Water → N-1,2-Benzisoxazol-3-yl-4-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine-1-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Chloro-3-phenyl-1,2,4-thiadiazole | HCID 32262 | — |
| 反応物 | N-1,2-Benzisoxazol-3-ylpiperazine-1-carboxamide trifluoroacetate | HCID 68778018 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-1,2-Benzisoxazol-3-yl-4-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine-1-carboxamide | HCID 11640074 | 65.6% |
反応手順
To a solution of 5-chloro-3-phenyl-1,2,4-thiadiazole (109 mg, 0.555 mmol) and N-1,2-benzisoxazol-3-ylpiperazine-1-carboxamide trifluoroacetate (200 mg, 0.555 mmol) in N,N-dimethylformamide (2 ml) was added triethylamine (0.389 ml, 2.78 mmol) at room temperature, and the mixture was stirred at room temperature for 2 hours. The reaction mixture was poured to water, and the precipitated solid was separated by filtration, which was recrystallized from a mixed solvent of ethyl acetate and tetrahydrofuran to give 148 mg (52.3%) of the desired product. mp 234-235° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07851473B2 |
| 出典データセット | uspto-grants-2010_12 |
| ORD ID | ord-616dd6a10ff140f79a7b30e0333d55be |
| 出典メモ | uspto-grants-2010_12 |