Hydrochloric Acid → HCID 136364256, compound

Temperature

64 °C

To a solution in which 2.09 g of ethyl 4-fluoro-2-methyl-3-oxopentanoate had been dissolved in 20 ml of methanol were added 4.59 g of a 28 % sodium methoxide methanol solution and 1.61 g of formamidine acetate, and the mixture was stirred under reflux (64° C.) for 3 hours. Then, the reaction mixture was cooled to 10° C. or lower, 2.5 g of conc. hydrochloric acid was added to the mixture and the resulting mixture was concentrated under reduced pressure. To the concentrated solution was added 50 ml of acetone, and the mixture was stirred at 60° C. for 10 minutes, and then insolubles were removed by filtration. The filtrate was concentrated under reduced pressure, and the concentrated solution was recrystallized from 10 ml of acetone to obtain 1.10 g of 6-(1-fluoroethyl)-5-methyl-4-pyrimidone (isolated yield: 59.2%).

1. temperatureThen, the reaction mixture was cooled to 10° C.
2. concentrationthe resulting mixture was concentrated under reduced pressure
3. additionTo the concentrated solution was added 50 ml of acetone
4. stirringthe mixture was stirred at 60° C. for 10 minutes
5. custominsolubles were removed by filtration
6. concentrationThe filtrate was concentrated under reduced pressure
7. customthe concentrated solution was recrystallized from 10 ml of acetone

ORD record

ord-54fef7828d7a4a9ab5774d15c787c2cd

Source dataset

uspto-grants-2002_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06340757B1