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Water → N-[4-(Acetylamino)phenyl]-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 | 2,2,2-Trichloroethyl[6-(acetylamino)pyridin-3-yl]carbamate | HCID 86245259 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | N-[4-(Acetylamino)phenyl]-4-[3-(3-thienyl)phenyl]piperazine-1-carboxamide | HCID 16113932 | 51.5% |
反応手順
A mixed solution of 2,2,2-trichloroethyl[6-(acetylamino)pyridin-3-yl]carbamate (147 mg, 0.450 mmol), 1-[3-(3-thienyl)phenyl]piperazine (100 mg, 0.409 mmol) and diisopropylethylamine (0.143 ml, 0.818 mmol) in dimethylsulfoxide (1.5 ml) was stirred at 70° C. for 15 hours. 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 85.5 mg (51.5%) 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-a3b717ebb86741f5af12ade3a8fca844 |
| 出典メモ | uspto-grants-2010_10 |