反应详情

A mixture of bicyclo[2.2.2]octane-2,3-dicarboxylic anhydride (541 mg, 3 mmol), 1-(4-aminobutyl)-4-(2-pyrimidinyl)piperazine (708 mg, 3 mmol) and pyridine (12.1 ml) was refluxed for 10 hours. The solvent was removed from the mixture under reduced pressure. The residue was extracted with chloroform and water. The chloroform layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to give crude crystals (1 g), which were treated with 6% hydrogen chloride/isopropanol. The solvent was removed to give N-[4-{4-(2-pyrimidinyl)-1-piperazinyl}-butyl]bicyclo[2.2.2]octane-2,3-dicarboximide hydrochloride (from ethanol). M.P. 198°-200° C.

1. temperaturewas refluxed for 10 hours
2. customThe solvent was removed from the mixture under reduced pressure
3. extractionThe residue was extracted with chloroform and water
4. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customto give crude crystals (1 g), which
7. customThe solvent was removed