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1-(3-Pentyl)piperazine → 4-(1-Ethylpropyl)piperazine-1-carboxylic Acid 3-trifluoromethylphenyl Ester Hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-(3-Pentyl)piperazine | HCID 2737116 | — |
| 反応物 | 3-(Trifluoromethyl)phenyl chloroformate | HCID 5057425 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(1-Ethylpropyl)piperazine-1-carboxylic Acid 3-trifluoromethylphenyl Ester Hydrochloride | HCID 69022763 | 86.7% |
反応手順
To a stirred mixture of 1-(1-ethylpropyl)piperazine (175p1, 1.0 mmol) and dry DCM (10 ml) was added 3-trifluoromethylphenyl chloroformate (250 mg, 1.1 mmol). The mixture was stirred overnight at room temperature and then diluted with DCM (50 ml). The reaction mixture was washed with 1 N NaOH (3×25 ml) and water (2×25 ml). The organic solution was concentrated and the residue was dissolved in a 0.5 N HCl solution (15 ml) and a small portion of acetonitrile. The acidic solution was concentrated and stirred with ethyl acetate (15 ml). The solid was isolated and dried to give 330 mg (86%) of the title compound as a solid. M.p. 260-261° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07279470B2 |
| 出典データセット | uspto-grants-2007_10 |
| ORD ID | ord-fd674f70440b4624b481b206cab96f30 |
| 出典メモ | uspto-grants-2007_10 |