Water → HCID 22097367, compound

Participants

Reaction Steps

3.7 g of 1-[5-methyl-1-(2-pyrimidinyl)-4-pyrazolyl]-3-[4-(2-chlorophenyl)-1-piperazinyl]-1-propanone hydrochloride was dissolved in 300 ml of methanol. After adding 1.25 g of sodium boron hydride, the obtained mixture was stirred at room temperature for 2 hours. To the reaction mixture was further added 0.6 g of sodium boron hydride followed by stirring for 2 hours. Under ice cooling, water was added to the reaction mixture and the methanol was removed by evaporation. The residue was extracted with chloroform and the extract was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. After evaporating the solvent, the residue was subjected to silica gel column chromatography and developed with a solvent mixture (chloroform/methanol, 30:1) to thereby give 1-[5-methyl-1-(2-pyrimidinyl)-4-pyrazolyl]-3-[4-(2-chlorophenyl-)1-piperazinyl]-1-propanol. Next, 16 ml of a 1N hydrochloric acid/ethanol solution was added to the product. After dissolving by heating, ether was further added thereto. The crystals thus precipitated were collected by filtration to thereby give 1.26 g of the title compound.

Provenance & Evidence