反应详情

温度

0 °C

A solution of 29C (0.9 g, 2.4 mmol) in DCM (20 mL) was treated with TFA (10 g, 88 mmol) and stirred at 0° C. for 4 h. The reaction mixture was concentrated and the residue was dissolved in aqueous NaHCO3 (sat.). The mixture was extracted three times with DCM and the organic solutions were filtered through a phase separator. The solvent was removed by evaporation. There was obtained 0.21 g (32%) of 29D as a colorless oil. 1H NMR (500 MHz, CDCl3): δ 2.28 (s, 3H), 2.28-2.68 (bm, 8H), 3.52 (s, 2H), 3.69-3.85 (m, 2H), 3.85-4.02 (m, 2H), 4.88-5.03 (m, 1H), 6.36-6.58 (m, 2H), 7.15-7.27 (m, 1H).

1. concentrationThe reaction mixture was concentrated
2. dissolutionthe residue was dissolved in aqueous NaHCO3 (sat.)
3. extractionThe mixture was extracted three times with DCM
4. filtrationthe organic solutions were filtered through a phase separator
5. customThe solvent was removed by evaporation