Water → 6-(1fluoroethyl)-4-pyrimidone

Participants

Reaction Conditions

Reaction Steps

To a solution in which 24.3 g of ethyl 4-fluoro-3-oxopentanoate had been dissolved in 330 ml of methanol were added 72.3 g of a 28 % sodium methoxide methanol solution and 15.6 g of formarnidine acetate, and the mixture was stirred at 50° C. for 3 hours. To the mixture was further added 7.81 g of formamidine acetate and after stirring the mixture at 50° C. for 4 hours, the mixture was cooled to 10° C. or lower. After cooling, 18.8 g of conc. sulfuric acid and 13.5 g of water were added to the reaction mixture. After stirring the mixture at 50° C. for 15 minutes, insolubles were removed by filtration and the filtrate was quantitated by the liquid chromatography internal standard method. As a result, 18.0 g of 6-(1-fluoroethyl)-4-pyrimidone was formed (yield: 84.6%).

Provenance & Evidence