反应详情

温度

70 °C

To a solution of N-[2-(3-cyano-5-fluorophenyl)-3-(4-hydroxyphenyl)-1-methylpropyl]-2-(5-trifluoromethyl-2-pyridyloxy)-2-methylpropanamide from Example 7, Step B (15 mg, 0.039 mmol) in 2 mL of dimethylformamide was added cesium carbonate (15 mg, 0.046 mmol) and 2-fluoroethyl methanesulfonate (20 uL, 0.16 mmol), and the reaction was stirred at 70° C. for 0.5 h. The resulting mixture was diluted with ether (20 mL), washed with water and brine and concentrated to dryness, and the residue was purified by flash column chromatography on silica gel eluted with 10 to 40% ethyl acetate in hexane to give N-{2-(3-cyano-5-fluorophenyl)-3-[4-(2-fluoroethoxy)phenyl]-1-methylpropyl}-2-(5-trifluoromethyl-2-pyridyloxy)-2-methylpropanamide. 1H NMR (500 MHz, CD3OD): PL 87 δ 8.27 (br s, 1H), 7.94 (dd, 1H), 7.48 (d, 1H), 7.73-7.32 (m, 3H), 7.04 (s, 1H), 6.64 (s, 4H) 4.68 (m, 1H), 4.59 (m, 1H), 4.25 (m, 1H), 4.11 (m, 1H), 4.04 (m, 1H), 3.02 (dd, 1H), 2.84 (m, 1H), 2.57 (dd, 1H), 1.75 (s, 3H), 1.73 (s, 3H), 0.80 (d, 3H). LC-MS: m/e 544 (M+H)+ (3.8 min).

1. washwashed with water and brine
2. concentrationconcentrated to dryness
3. customthe residue was purified by flash column chromatography on silica gel
4. washeluted with 10 to 40% ethyl acetate in hexane