反应详情

A mixture of compound 1A (4.56 g, 16.0 mmol) and lithium hydroxide monohydrate (2.0 g, 48.0 mmol) in MeOH (32 mL), THF (32 mL) and water (16 mL) was heated to reflux for 0.5 h. HPLC indicated that the reaction was complete. The organic solvents were removed under reduced pressure, and the aqueous residue was diluted with water. The pH was adjusted to 3.0 with 6N aqueous hydrochloric acid. The resulting precipitate was collected by vacuum filtration, rinsed with water and dried under reduced pressure to provide 3.95 g (96%) of 1B as a bright yellow solid. HPLC retention time=2.75 min. (Condition A) and LC/MS M++1=258+.

1. temperaturewas heated
2. temperatureto reflux for 0.5 h
3. customThe organic solvents were removed under reduced pressure
4. additionthe aqueous residue was diluted with water
5. filtrationThe resulting precipitate was collected by vacuum filtration
6. washrinsed with water
7. customdried under reduced pressure