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Water → N-1,2-Benzisoxazol-3-yl-4-[3-(4-chlorophenyl)-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-(4-chlorophenyl)-1,2,4-thiadiazole | HCID 46318464 | — |
| 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-(4-chlorophenyl)-1,2,4-thiadiazol-5-yl]piperazine-1-carboxamide | HCID 68780033 | 34.7% |
反応手順
To a solution of 5-chloro-3-(4-chlorophenyl)-1,2,4-thiadiazole (179 mg, 0.555 mmol) and N-1,2-benzisoxazol-3-ylpiperazine-1-carboxamide trifluoroacetate (200 mg, 0.555 mmol) in 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 85.0 mg (34.7%) of the desired product.
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-77e4b5a0bc4d4ceb872092e1c8aae553 |
| 出典メモ | uspto-grants-2010_12 |