反应详情

A solution of 7B (2.1 g, 5.47 mmol) in DCM (20 mL) was treated with TFA (10 g, 88 mmol) and stirred at RT for 2 h. The reaction mixture was concentrated and the residue was dissolved in aqueous NaHCO3 (sat.) and extracted several times with DCM and 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 1.0 g (66%) of 7C as a colorless oil. 1H NMR (500 MHz, CDCl3): δ 2.40-2.53 (m, 4H), 3.47 (s, 2H), 3.66-3.74 (m, 4H), 3.78 (s, 3H), 3.77-3.84 (m, 2H), 3.89-3.97 (m, 2H), 4.94-5.04 (m, 1H), 6.23 (d, 1H), 6.37 (s, 1H), 7.19 (d, 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