反应详情

温度

100 °C

A suspension of the product of Step 228c (181 mg, 0.550 mmol), 2-fluoro-5-(trifluoromethyl)pyridine (108 mg, 0.655 mmol), and K2CO3 (152 mg, 1.10 mmol) in anhydrous DMF (4 mL) was heated at 100° C. under nitrogen for 3 h. The reaction mixture was cooled to rt, diluted with EtOAc (100 mL), washed with 10% aq. LiCl (3×50 mL), dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel (0% to 100% EtOAc/hexanes) then lyophilized from acetonitrile/water (2:1) to afford the title compound as a white solid (220 mg, 84%). 1H NMR (500 MHz, CDCl3) δ 8.95-6.05 (m, 10H), 5.25-2.85 (m, 5H), 2.15-0.75 (m, 8H); ESI MS (M+H) 474.

1. temperatureThe reaction mixture was cooled to rt
2. washwashed with 10% aq. LiCl (3×50 mL)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by flash column chromatography on silica gel (0% to 100% EtOAc/hexanes)