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Laurolactam → n-(cis-2-Phenyl-cyclopentyl) azacyclotridecan-2-imine-hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Laurolactam | HCID 13690 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | rac-(1R,2R)-2-phenylcyclopentan-1-amine hydrochloride | HCID 70051154 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | n-(cis-2-Phenyl-cyclopentyl) azacyclotridecan-2-imine-hydrochloride | HCID 136349517 | — |
反応手順
To 21.7 g of 2-azacyclotridecanone in 200 ml of dry benzene was added dropwise 15.3 g of phosphorus oxychloride. The mixture was stirred at room temperature for 4 hours after which 19.8 g of cis-2-phenylcyclopentylamine hydrochloride was added. The reaction mixture was stirred at room temperature for 2 hours and refluxed for 24 hours. The resulting homogeneous solution was washed with 2 N NaOH, 2 N HCl and saturated NaCl solution, dried over sodium sulfate and the solvent evaporated. The resulting oily product crystallized from acetone and was recrystallized from methanol-acetone to give the desired product, M.P. 156°-159° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04153235 |
| 出典データセット | uspto-grants-1979_05 |
| ORD ID | ord-762009176f41401383768f2958878274 |
| 出典メモ | uspto-grants-1979_05 |