反应详情

Compound 2 (10 g, 52.5 mmol) was dissolved in MeCN (150 mL) and NIS (14.2 g, 62.9 mmol) was added. The solution was heated to reflux for 5 h and cooled to room temperature. The solvent was evaporated and the residue was dissolved in EtOAc. The organics were washed with sat. NaHCO3 and sat. NaS2O3, dried (MgSO4), filtered and concentrated to give the title compound as a white solid. 1H NMR (CDCl3) δ 4.04 (s, 3H), 2.54 (s, 3H); LCMS 2.64 min, 317 (M+H).

1. temperatureThe solution was heated
2. temperatureto reflux for 5 h
3. customThe solvent was evaporated
4. dissolutionthe residue was dissolved in EtOAc
5. washThe organics were washed with sat. NaHCO3 and sat. NaS2O3
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated