Benzoyl chloride → Benzamide, N-(5-methyl-1H-pyrazol-3-yl)-

Participants

Reaction Steps

103 g (1 mol) of calcium carbonate were added with stirring to a solution of 50 g (0.5 mol) of 3-amino-5-methyl-1H-pyrazole in 100 cm3 of dioxane. 73 cm3 (0.6 mol) of benzoyl chloride were added dropwise to this solution at 65° C. The temperature was brought to 80° C. and maintained for 1 hour. The solution was subsequently brought back to 10° C. A beige solid formed during the reaction was pulled dry on sintered glass and was then taken up again with stirring in 400 cm3 of methanol. The solution was filtered and the filtrate was concentrated under vacuum. A beige solid crystallized and was pulled dry on sintered glass and then washed with 50 cm3 of isopropyl ether. After drying under vacuum at 40° C., 25 g of the expected product were obtained in the form of beige crystals, the melting point of which was between 218 and 220° C.

Provenance & Evidence