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Triethylamine → N-[3-[4-(2-Methoxyphenyl)-1-piperazinyl]propyl]-2-benzofurancarboxamide Dihydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Benzofurancarbonyl chloride | HCID 38949 | — |
| 反応物 | 1-(3-Aminopropyl)-4-(2-methoxyphenyl)piperazine | HCID 10467259 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-[3-[4-(2-Methoxyphenyl)-1-piperazinyl]propyl]-2-benzofurancarboxamide Dihydrochloride | HCID 18995783 | — |
反応手順
To a stirred solution of [4-(2-methoxyphenyl)piperazinyl]propylamine (1.0 g, 0.04 mol) in 50 mL of methylene dichloride, benzofurane-2-carboxylic acid chloride (1.01 g, 0.0056 mol) and triethylamine (1 g, 0.01 mol) were added. Stirring was continued at room temperature overnight. The methylene chloride solution was washed with water, dried over anhydrous sodium sulfate and evaporated under reduced pressure. The remaining residue was subjected to preparative HPLC using silica gel column and ethyl acetate as the eluent. The title compound was separated and converted to the dihydrochloride salt with ethanolic HCl (0.9 g), m.p. 228°-232° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05482940 |
| 出典データセット | uspto-grants-1996_01 |
| ORD ID | ord-5237be46d3504ae4a458eac030c49b0c |
| 出典メモ | uspto-grants-1996_01 |