反应详情

温度

70 °C

To a solution of the title compound from Example 330 Step A (300 mg, 1.94 mmol) in acetonitrile (4 mL) was added ethyl 2-(ethoxymethylene)-4,4,4-trifluoro-3-oxobutyrate (0.284 mL, 1.94 mmol) followed by TEA (0.271 mL, 1.94 mmol), and the mixture was heated at 70° C. After 16 h, the reaction mixture was concentrated in vacuo. Purification by flash chromatography on silica gel (0 to 65% EtOAc in hexanes) provided the title compound as a yellow oil: LCMS m/z 320.85 [M+H]+; 1H NMR (500 MHz, CD3OD) δ 8.03 (t, J=7.9 Hz, 1H), 7.77 (d, J=7.7 Hz, 1H), 7.64 (d, J=8.0 Hz, 1H), 4.55 (q, J=7.2 Hz, 2H), 1.49 (t, J=7.2 Hz, 3H).

1. concentrationthe reaction mixture was concentrated in vacuo
2. customPurification by flash chromatography on silica gel (0 to 65% EtOAc in hexanes)