Lithium iodide → HCID 66693235, compound

To a stirred solution of 1,6-dihydro-6-oxo-1,2-diphenyl-5-pyrimidinecarboxylic acid ethyl ester (i.e. Step B product (A)) (2.30 g, 7.18 mmol) in pyridine (15 mL) was added lithium iodide (2.46 g, 18.0 mmol). The reaction mixture was heated to reflux with stirring for 24 h. The reaction mixture was concentrated under reduced pressure. To the resulting residue was added water (10 mL) followed by 1 N hydrochloric acid until the pH was 7. The solution was filtered though Celite® diatomaceous filter aid. The filtrate was acidified with 1 N hydrochloric acid until the pH was 1, and the mixture was extracted with dichloromethane. The organic layer was dried (MgSO4) and concentrated under reduced pressure to afford a solid, which was washed with diethyl ether and dried under reduced pressure to afford the title product as a white solid (1.40 g).

1. temperatureThe reaction mixture was heated
2. temperatureto reflux
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. additionTo the resulting residue was added water (10 mL)
5. filtrationThe solution was filtered though Celite® diatomaceous filter aid
6. extractionthe mixture was extracted with dichloromethane
7. dry with materialThe organic layer was dried (MgSO4)
8. concentrationconcentrated under reduced pressure
9. customto afford a solid, which
10. washwas washed with diethyl ether
11. customdried under reduced pressure

ORD record

ord-c83f71cd8d0b4773be3f5d8e3239aadc

Source dataset

uspto-grants-2015_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09187432B2