反应详情

159 (850 mg) was dissolved in 4 ml of DCM and 4 ml of TFA was added then the reaction mixture was let 1 h at room temperature. The reaction mixture is concentrated and 50 ml of AcOEt are added. The organic phase are washed with saturated NaHCO3 and brine then dried over Na2SO4, filtered and concentrated to afford 160 as a white solid (540 mg, 86%). 1H NMR (DMSO): δ 1.26 (t, 3H, J=6.5 Hz), 1.89 (s, 2H), 2.89 (dd, 1H, J=13.1, 6.1 Hz), 2.97 (dd, 1H, J=13.1, 6.1 Hz), 3.68 (t, 1H, J=6.1 Hz), 4.16 (q, 2H, J=6.5 Hz), 5.21 (s, 2H), 6.90 (d, 1H, J=7.6 Hz), 6.99 (s, 2H), 7.32 (t, 1H, J=7.8 Hz), 7.47 (m, 1H), 7.53 (t, 2H, J=7.0 Hz), 7.58 (d, 2H, J=7.6 Hz).

1. concentrationThe reaction mixture is concentrated
2. addition50 ml of AcOEt are added
3. washThe organic phase are washed with saturated NaHCO3 and brine
4. dry with materialthen dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated