反应详情

To a solution of Intermediate 46 (2.9 g, 13.98 mmol) in methanol (22.6 mL) was added dropwise sulphuric acid (0.4 mL, 6.94 mmol) during 15 minutes at 0° C. The resulting reaction mixture was refluxed for 2 hours. The solvent was removed under reduced pressure and the crude was partitioned between ethyl acetate and water. The organic layer was washed with a solution of sodium hydrogen carbonate (4%), water and brine. The solvent was removed under reduced pressure and the title compound was obtained as a red oil (2.9 g, 95%) and was used in the next step without further purification.

1. customThe resulting reaction mixture
2. temperaturewas refluxed for 2 hours
3. customThe solvent was removed under reduced pressure
4. customthe crude was partitioned between ethyl acetate and water
5. washThe organic layer was washed with a solution of sodium hydrogen carbonate (4%), water and brine
6. customThe solvent was removed under reduced pressure