Hydrochloric Acid → HCID 135627622, compound

Temperature

50 °C

To a solution in which 5.52 g of ethyl 4-fluoro-4-methyl-3-oxopentanoate had been dissolved in 20 ml of methanol were added 11.6 g of a 28 % sodium methoxide methanol solution and 4.0 g of formamidine acetate, and the mixture was stirred at 50° C. for 6 hours. The mixture was cooled to 10° C. or lower, and 7.1 g of conc. hydrochloric acid was added to the reaction mixture and the reaction mixture was concentrated under reduced pressure. To the concentrated solution was added 100 ml of acetone, and the resulting mixture was stirred at 60° C. for 30 minutes and then, insolubles were removed by filtration. The filtrate was concentrated under reduced pressure and the concentrated solution was recrystallized from 20 ml of acetone to obtain 2.0 g of 6-(1-fluoro-1-methylethyl)-4-pyrimidone (isolated yield: 64.0%).

1. temperatureThe mixture was cooled to 10° C.
2. concentrationthe reaction mixture was concentrated under reduced pressure
3. additionTo the concentrated solution was added 100 ml of acetone
4. stirringthe resulting mixture was stirred at 60° C. for 30 minutes
5. custominsolubles were removed by filtration
6. concentrationThe filtrate was concentrated under reduced pressure
7. customthe concentrated solution was recrystallized from 20 ml of acetone

ORD record

ord-d7d08066998341c3afa225c5fae48bc3

Source dataset

uspto-grants-2002_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06340757B1