反应详情

温度

55 °C

The product from Step 4B (6 g, 0.017 mol) was dissolved in DMF (40 ml) at room temperature under nitrogen. Caesium carbonate (8.2 g, 0.025 mol) was added followed by trifluoroethyl iodide (8.8 g, 0.025 mol) and the mixture stirred at 55° C. for 16 hr. The reaction mixture was taken up in ethyl acetate/water, the organic layer washed (water, brine), dried (MgSO4) and evaporated in vacuo. Purification by chromatography (SiO2, ethyl acetate/dichloromethane) afforded the product as a white solid (2.6 g, 35%). (1H NMR, CDCl3) δ 3.68–3.83 (11H, m), 4.13–4.17 (1H, m), 4.72 (1H, S d, J=13.6 Hz), 4.84–4.88 (1H, m) 5.04 (1H, d, J=13.6Hz), 6.13 (2H, s), 7.18 (1H, d, J=8.3 Hz), 7.32–7.50 (2H, m), 7.96 (1H, m).

1. washthe organic layer washed (water, brine)
2. dry with materialdried (MgSO4)
3. customevaporated in vacuo
4. customPurification by chromatography (SiO2, ethyl acetate/dichloromethane)