1H-Pyrazol-5-ol, 3-methyl-1-phenyl- → HCID 18457995, compound

Participants

Reaction Steps

3-Methyl-1-phenylpyrazol-5-one (5 g; 0.029 mole) was placed in a flask equipped with a stirrer and reflux condenser. Dry and distilled dioxane (40 ml) was added by warming and to the clear solution calcium hydroxide (6.4 g; 0.086 mole) was added followed by drop wise addition of tert-butylacetyl chloride (4.8 ml; 0.034 mole). The mixture was heated to reflux for 4 hours and then poured into 2M HCl (200 ml) to decompose the calcium complex. A light brown precipitate formed immediately, which was filtered off under suction after refrigerating overnight. The product washed with water and dried under vacuum at 50° C. The product was recrystallised from methanol to give an off-white crystalline solid, m.p 85-86° C.; 6.8 g (82%).

Provenance & Evidence