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Hydrochloric Acid → 1-(4-Chlorophenyl)-2-[(3-oxo-1-azabicyclo[2.2.2]oct-2-yl)methyl]-1,3-butanedione hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1-(4-Chlorophenyl)butane-1,3-dione | HCID 238083 | — |
| 反応物 | 2-Methylene-3-quinuclidone | HCID 322973 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 1-(4-Chlorophenyl)-2-[(3-oxo-1-azabicyclo[2.2.2]oct-2-yl)methyl]-1,3-butanedione hydrochloride | HCID 13971538 | — |
反応手順
To a solution of 93.10 g (0.47 mole) 1-(4-chlorophenyl)-1,3-butanedione in 500 ml acetone add 60.0 g (0.39 mole) 2-methylene-3-quinuclidinone. Stir the solution at reflux for about 24 hours. Follow the progress of the reaction by thin-layer chromatography on silica gel (EtOAc:MeOH, 9:1). At the completion of the reaction, chill the solution in an ice/water bath. Acidify dropwise with 35 ml concentrated hydrochloric acid to precipitate the product. Collect the precipitate by filtration to obtain the title compound as a mixture of diastereomers.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04599344 |
| 出典データセット | uspto-grants-1986_07 |
| ORD ID | ord-e708001b140e4ae7a59fe77869336848 |
| 出典メモ | uspto-grants-1986_07 |