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O-Xylene → 3-[4-[4-(6-Chloro-2-pyrazinyl)-1-piperazinyl]butyl]-8,8-dimethyl-3-azabicyclo[3.2.1]octane-2,4-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | O-Xylene | HCID 7237 | — |
| 反応物 | 4-[4-(6-Chloropyrazin-2-yl)piperazin-1-yl]butan-1-amine | HCID 14086526 | — |
| 反応物 | 8,8-Dimethyl-3-oxabicyclo(3.2.1)octane-2,4-dione | HCID 19797203 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-[4-[4-(6-Chloro-2-pyrazinyl)-1-piperazinyl]butyl]-8,8-dimethyl-3-azabicyclo[3.2.1]octane-2,4-dione | HCID 14156383 | — |
反応手順
2,2-Dimethylcyclopentane-1,3-dicarboxylic anhydride (1.68 g., 10 mmole) and 1-(4-aminobutyl)-4-(6-chloro-2-pyrazinyl)piperazine (2.97 g., 11 mmole) were combined in 500 ml. of xylene and refluxed for 48 hours with Dean-Stark water removal. Concentration in vacuum, column chromatography on 100 g. of silica gel with chloroform, and recrystallization from 50 ml. of isopropanol with addition of 4N isopropanolic HCl gave 0.55 g. of the title compound as the monohydrochloride; m.p. 210° C. (d).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04748240 |
| 出典データセット | uspto-grants-1988_05 |
| ORD ID | ord-759e9be378344115804eb0877f7c45f7 |
| 出典メモ | uspto-grants-1988_05 |