化工社化工社 化学情報印刷レポート · 研究参考用
Water → N-Pyridin-3-yl-4-[3-(3-thienyl)phenyl]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 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1-[3-(3-Thienyl)phenyl]piperazine | HCID 58985140 | — |
| 反応物 | HCID 68575380 | HCID 68575380 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | N-Pyridin-3-yl-4-[3-(3-thienyl)phenyl]piperazine-1-carboxamide | HCID 16114127 | 37.4% |
反応手順
A mixed solution of 2,2,2-trichloroethyl pyridin-3-ylcarbamate (303 mg, 1.13 mmol), 1-[3-(3-thienyl)phenyl]piperazine (250 mg, 1.02 mmol) and diisopropylethylamine (0.356 ml, 2.05 mmol) in dimethylsulfoxide (3.5 ml) was stirred at 70° C. for 3 days. Water was poured into the reaction solution, and extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate, and the solvent was distilled away under reduce pressure. The residue was purified by silica gel column chromatography (ethyl acetate), and recrystallized from a mixed solvent of hexane and tetrahydrofuran to give the titled compound 139 mg (37.3%) as solid product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07812025B2 |
| 出典データセット | uspto-grants-2010_10 |
| ORD ID | ord-a0e2c83ccadb4bdf9c927cdbe862ecf0 |
| 出典メモ | uspto-grants-2010_10 |