Sodium Iodide → N-(4-(difluoromethoxy)phenyl)-7-(3-(trifluoromethyl)pyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine

Temperatur

150 °C

In a 5 mL microwave vial was combined 4-chloro-7-(3-(trifluoromethyl)pyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine (0.113 g, 0.000356 mol), 4-(trifluoromethoxy)aniline (0.0964 mL, 0.000711 mol), acetonitrile (2 mL, 0.04 mol), and sodium iodide (0.00533 g, 0.0000356 mol). The mixture was heated at at 150° C. for 10 minutes and reduced in vacuo. The remaining solid was taken up in ethyl acetate (10 mL) and washed with saturated sodium bicarbonate (2×10 mL) and water (1×10 mL). The organic layer was dried over magnesium sulfate and reduced in vacuo to yield an off white solid. The mixture was purified by flash chromatography using an ethyl acetate:hexanes (0-50%) gradient to yield the desired product as an off white solid (0.052 g).

1. washwashed with saturated sodium bicarbonate (2×10 mL) and water (1×10 mL)
2. dry with materialThe organic layer was dried over magnesium sulfate
3. customto yield an off white solid
4. customThe mixture was purified by flash chromatography

ORD-Eintrag

ord-255d22f923ba4c4184747a58601e3f4a

Quelldatensatz

uspto-grants-2007_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07312330B2