Formaldehyde → 1-[5-Methyl-1-(2-pyrimidinyl)-4-pyrazolyl]-3-[4-(4-methoxyphenyl)-1-piperazinyl]-1-propanone hydrochloride

Participants

Reaction Steps

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.

Provenance & Evidence