関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Adamantanecarbonyl chloride | HCID 98915 | — |
| 反応物 | 1-(3-Aminopropyl)-4-(2-methoxyphenyl)piperazine | HCID 10467259 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 131716829 | HCID 131716829 | — |
反応手順
To a stirred solution of [4-(2-methoxyphenyl)piperazinyl]propylamine (2.5 g, 0.01 mol) in 50 mL of methylene chloride, adamantane-1-carboxylic acid chloride (2.02 g, 0.010 mol) and triethylamine (2 g, 0.02 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. In repeated preparations, the residue was dissolved in ethyl acetate (10 mL) and subjected to flash chromatography using a 9 inch column of silica gel and ethyl acetate as the eluent. The title compound (TLC Rf =0.53 in 30% methanol/ethyl acetate system) was separated and converted to the hydrochloride hemihydrate salt with ethanolic HCl (2.3 g), m.p. 186°-190° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05482940 |
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| 出典データセット | uspto-grants-1996_01 |
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| ORD ID | ord-42ca4160030642aa9ee47a74f863fa6d |
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| 出典メモ | uspto-grants-1996_01 |
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