Potassium Carbonate → HCID 178488429, Verbindung

A mixture of 2-amino-6-bromo-8-(cis-4-(2-hydroxyethoxy)cyclohexyl)-4-methylpyrido[2,3-d]pyrimidin-7(8H)-one (50 mg, 0.13 mmol), potassium carbonate (52 mg, 0.38 mmol), and 2-methoxy-5-pyridine boronic acid (38 mg, 0.25 mmol) in 5:1 dimethylformade:water (1.3 mL) was bubbled with argon for 5 minutes. To the mixture was added bis(tripehnylphosphine) palladium (II) chloride (9 mg, 0.13 mmol) and the microwave vial was immediately sealed and the mixture was bubbled again with argon. After heating for 20 min at 100° C. in the microwave, the mixture was concentrated in vacuo. The residue was dissolved in CHCl3 (60 mL) and washed with water (10 mL) and brine (10 mL). The organic layer was dried (Na2SO4), filtered and concentrated. The crude product was purified by flash chromatography eluting with chloroform/7 N ammonia in methanol (0-5%) to afford the title compound (50 mg, 93%).

1. customwater (1.3 mL) was bubbled with argon for 5 minutes
2. customthe microwave vial was immediately sealed
3. customthe mixture was bubbled again with argon
4. concentrationthe mixture was concentrated in vacuo
5. dissolutionThe residue was dissolved in CHCl3 (60 mL)
6. washwashed with water (10 mL) and brine (10 mL)
7. dry with materialThe organic layer was dried (Na2SO4)
8. filtrationfiltered
9. concentrationconcentrated
10. customThe crude product was purified by flash chromatography
11. washeluting with chloroform/7 N ammonia in methanol (0-5%)

ORD-Eintrag

ord-1c561698d2d44b5685c50d9348be7067

Quelldatensatz

uspto-grants-2010_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07696213B2