Hydrochloric Acid → HCID 135743677, compound

Temperature

40 °C

62.10 g (1150 mmol) of sodium methoxide are added to a mixture of 340 mL (2230 mmol) of diethyl malonate heated to 40° C. The mixture is heated at 100° C. until a clear solution is obtained. 59.50 g (360 mmol) of 4-trifluoromethyl-1,4,5,6-tetrahydropyrimidin-2-ylamine dissolved in 100 mL of methanol are then added to the reaction medium. The mixture obtained is maintained at 100° C. for 1 hour and then cooled to room temperature overnight. The reaction mixture is evaporated to dryness under reduced pressure. The residue obtained is taken up in 250 mL of water. 12 N hydrochloric acid is added to the thick suspension obtained, to pH=5-6. The suspension obtained is filtered through a sinter funnel and the insoluble matter is rinsed with acetonitrile to give 68.10 g of 2-hydroxy-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one in the form of a yellow solid, the characteristics of which are as follows:

1. temperatureThe mixture is heated at 100° C. until a clear solution
2. customis obtained
3. additionare then added to the reaction medium
4. customThe mixture obtained
5. temperatureis maintained at 100° C. for 1 hour
6. temperaturecooled to room temperature overnight
7. customThe reaction mixture is evaporated to dryness under reduced pressure
8. customThe residue obtained
9. customobtained, to pH=5-6
10. customThe suspension obtained
11. filtrationis filtered through a sinter funnel
12. washthe insoluble matter is rinsed with acetonitrile

ORD record

ord-9991b48f336749a99631c979453aea5f

Source dataset

uspto-grants-2016_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09321790B2