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Triethylamine → N-[2-[4-(2-Pyrimidinyl)-1-piperazinyl]ethyl]tricyclo[3,3,1,13,7]decane-1-carboxamide Dihydrochloride Hydrate
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-Piperazineethanamine, 4-(2-pyrimidinyl)- | HCID 13885358 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-[2-[4-(2-Pyrimidinyl)-1-piperazinyl]ethyl]tricyclo[3,3,1,13,7]decane-1-carboxamide Dihydrochloride Hydrate | HCID 131717305 | — |
反応手順
To a stirred solution of [4-(2-pyrimidinyl)piperazinyl]ethylamine (2.0 g, 0.01 mol) in 50 mL of methylene chloride, adamantane-1-carboxylic acid chloride (3.6 g, 0.018 mol) and triethylamine (2.9 g, 0.015 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 dissolved in ethyl acetate (10 mL) and subjected to column chromatography using silica gel and ethyl acetate as the eluent. The title compound was separated and converted to the dihydrochloride hydrate salt with ethanolic HCl (2.4 g), m.p. 237°-239° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05106849 |
| 出典データセット | uspto-grants-1992_04 |
| ORD ID | ord-9112aec6659c4a82a2032bb1827e884b |
| 出典メモ | uspto-grants-1992_04 |