反应详情

1.0 g of 1-(2-pyrimidinyl)-4-acetyl-5-methyl-pyrazole was dissolved in 50 ml of ethanol. After adding 1.3 g of 1-(4-methoxyphenyl)piperazine dihydrochloride and 0.8 g of paraformaldehyde, the mixture was heated under reflux for 24 hours. Further, 0.8 g of paraformaldehyde was added and the resulting mixture was heated under reflux for additional 48 hours. Then the reaction mixture was concentrated and neutralized by adding a saturated aqueous solution of sodium hydrogencarbonate. After extracting with chloroform, the extract was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. After evaporating the solvent, the residue thus obtained was purified by silica gel column chromatography (chloroform:methanol=50:1), converted into hydrochloride by adding a 1N hydrochloric acid/ethanol solution and then recrystallized from ethanol. Thus 1.1 g of the title compound was obtained in the form of a pale yellow powder.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 24 hours
3. temperaturethe resulting mixture was heated
4. temperatureunder reflux for additional 48 hours
5. concentrationThen the reaction mixture was concentrated
6. additionby adding a saturated aqueous solution of sodium hydrogencarbonate
7. extractionAfter extracting with chloroform
8. washthe extract was washed with a saturated aqueous solution of sodium chloride
9. dry with materialdried over anhydrous sodium sulfate
10. customAfter evaporating the solvent
11. customthe residue thus obtained
12. customwas purified by silica gel column chromatography (chloroform:methanol=50:1)
13. additionby adding a 1N hydrochloric acid/ethanol solution
14. customrecrystallized from ethanol