甲基 4-氟-3-氧代戊酸乙酯

反应条件: temp:32.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a liquid in which 1.31 g of a 62.8% sodium hydride had been suspended in 10 ml of tetrahydrofaran was added dropwise a mixed solution of 2.00 g of methyl 2-fluoropropionate and 2.10 g of methyl acetate over 10 minutes, and the mixture was then heated at 30 to 35° C. for 4 hours. After completion of the reaction, the reaction mixture was cooled to room temperature, neutralized with 1N-hydrochloric acid, and subjected to liquid separation. When the organic layer was quantitated by the gas chromatography internal standard method. As a result, it was found that 2.57 g of methyl 4-fluoro-3-oxopentanoate was formed (yield: 92%). When this organic layer was concentrated under reduced pressure and then distilled under reduced pressure, 2.03 g of methyl 4-fluoro-3-oxopentanoate could be obtained. After completion of the reaction the reaction mixture was cooled to room temperature subjected to liquid separation was formed (yield: 92%) When this organic layer was concentrated under reduced pressure distilled under reduced pressure, 2.03 g of methyl 4-fluoro-3-oxopentanoate could be obtained

反应条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution in which 9.33 g of methyl 4-fluoro-3-oxopentanoate had been dissolved in 115 ml of methanol were successively added 36.5 g of a 28% sodium methoxide methanol solution and 9.84 g of formamidine acetate at room temperature, and the mixture was stirred at 40° C. for 12 hours. To the mixture was further added 0.66 g of formamidine acetate and after stirring the mixture at 50° C. for 2 hours, the mixture was cooled to 10° C. or lower. After cooling, a mixture of 9.51 g of conc. sulfuric acid and 8.5 g of water was added to the reaction mixture. After stirring the mixture at 50° C. for 30 minutes, insolubles were removed by filtration and the filtrate was quantitated by the liquid chromatography internal standard method. As a result, 7.99 g of 6-(1-fluoroethyl)-4-pyrimidone was found to be formed (yield: 89.2%). The filtrate was concentrated under reduced pressure and the concentrated solution was recrystallized from 40 ml of 2-propanol to obtain 5.82 g of 6-(1-fluoroethyl)-4-pyrimidone. at room temperature after stirring the mixture at 50° C. for 2 hours the mixture was cooled to 10° C. After cooling was added to the reaction mixture After stirring the mixture at 50° C. for 30 minutes insolubles were removed by filtration to be formed (yield: 89.2%) The filtrate was concentrated under reduced pressure the concentrated solution was recrystallized from 40 ml of 2-propanol