反应详情

温度

0 °C

A solution of 9B (2.18 g, 5.81 mmol) in DCM (40 mL) was treated with TFA (10 g, 88 mmol) and stirred at 0° C. for 3 h. The reaction mixture was concentrated and the residue was dissolved in aqueous NaHCO3 (sat.) and extracted several times with DCM. The organic solutions were filtered through a phase separator. The solvent was removed by evaporation and the residue was purified by column chromatography on SiO2 using 10% triethylamine and 10% MeOH in EtOAc as eluent. There was obtained 1.44 g (90%) of 9C as a colorless oil. 1H NMR (500 MHz, CDCl3): δ 2.22 (s, 3H), 2.28 (s, 3H), 2.27-2.70 (bm, 8H), 3.40 (s, 2H), 3.75-3.85 (m, 2H), 3.88-3.98 (m, 2H), 4.92-5.02 (m, 1H), 6.43 (d, 1H), 7.01 (d, 1H), 7.09 (s, 1H).

1. concentrationThe reaction mixture was concentrated
2. dissolutionthe residue was dissolved in aqueous NaHCO3 (sat.)
3. extractionextracted several times with DCM
4. filtrationThe organic solutions were filtered through a phase separator
5. customThe solvent was removed by evaporation
6. customthe residue was purified by column chromatography on SiO2 using 10% triethylamine and 10% MeOH in EtOAc as eluent