Phosphorus oxychloride → HCID 57447453, compound

Participants

Reaction Conditions

Reaction Steps

0.57 g of 5-(4-chlorophenyl)-4-(3-chloro-2-pyrazinyl)-6-methyl-2H-pyridazin-3-one and 6 g of phosphorus oxychloride were mixed. The mixture was stirred for 2 hours on an oil bath of 110° C. The reaction mixture was allowed to cool to room temperature, then, concentrated under reduced pressure. To the resultant residue were added ethyl acetate and ice-cooled sodium bicarbonate water. The mixture was stirred for about 5 minutes at room temperature, then, liquid-separated. The organic layer was washed with brine, and dried over anhydrous magnesium sulfate, then, concentrated under reduced pressure. 0.60 g of the resultant residue was subjected to silica gel column chromatography, to obtain 0.49 g of 3-chloro-5-(4-chlorophenyl)-4-(3-chloro-2-pyrazinyl)-6-methylpyridazine (hereinafter, described as compound (12) of the present invention.).

Provenance & Evidence