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O-Xylene → 3-[4-[4-(2-Quinolyl)-1-piperazinyl]butyl]-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 | 1,3-Cyclopentanedicarboxylic acid | HCID 107216 | — |
| 反応物 | 1-(4-Aminobutyl)-4-(2-quinolyl)piperazine | HCID 21243703 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-[4-[4-(2-Quinolyl)-1-piperazinyl]butyl]-3-azabicyclo[3.2.1]octane-2,4-dione | HCID 14156365 | — |
反応手順
1,3-Cyclopentane dicarboxylic acid (1.6 g., 10 mmole) and 1-(4-aminobutyl)-4-(2-quinolyl)piperazine (2.8 g., 10 mmole) were combined in 200 ml. of xylene and refluxed for 24 hours with water removal via a Dean-Stark trap. The solvent was then removed in vacuum and the residue redissolved in chloroform and filtered through 75 g. of silica gel. The column was rinsed with 5% ethanol/chloroform and the product-containing fractions were combined and evaporated. The residue was recrystallized from isopropanol with the addition of 4N isopropanolic HCl to give 820 mg. of the title compound as the dihydrochloride hemihydrate; m.p. 240°-242° C.
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-b085f95e938f4d4f9b60dc63473ae7dd |
| 出典メモ | uspto-grants-1988_05 |