Sulfuric Acid → HCID 21270742, compound

Participants

Reaction Steps

3.70 ml of concentrated sulphuric acid are added dropwise during 1 minute to a solution of 3.80 g of 1-(4-chloro-2-fluoro-5-isopropoxyphenyl) -2-methoxy-4-trifluoromethyl-6(1H)-pyrimidinone (see Example 4, 2nd part) in 10 ml of methylene chloride while stirring and cooling at room temperature. The reaction mixture is stirred at room temperature for 3 hours and poured on to 15 g of ice. The organic phase is separated and the aqueous phase is extracted twice with 5 ml of methylene chloride each time and the combined organic phases are washed twice with 10 ml of water each time. The methylene chloride solution is subsequently dried over anhydrous sodium sulphate and evaporated to dryness under reduced pressure. The residue is recrystallized from diethyl ether/n-hexane. There is obtained 1-(4-chloro-2-fluoro-5-hydroxyphenyl)-2-methoxy-4-trifluoromethyl-6(1H)-pyrimidinone, m.p. 147°-149° C.

Provenance & Evidence