反应详情

To a solution of title compound 90 (9.32 g, 35.4 mmol) in MeOH (30 mL) and water (5 mL) was added ammonium chloride (3.79 g, 70.8 mmol) and zinc chloride (20.83 g, 319 mmol) and the reaction mixture was heated to reflux for 2 hours. The mixture was cooled to room temperature and filtered and the solvent removed. The residue was diluted with ethyl acetate and water and the organic phase was washed well with water, dried over Na2SO4, filtered and concentrated to afford title compound 91 (8.3 g, 100%). LRMS (ESI): (calc) 233.09 (found) 234.1 (MH)+.

1. temperaturethe reaction mixture was heated
2. temperatureto reflux for 2 hours
3. filtrationfiltered
4. customthe solvent removed
5. additionThe residue was diluted with ethyl acetate and water
6. washthe organic phase was washed well with water
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated