反应详情

The compound of Example 1 (0.442g, 0.740 mmol) was dissolved in 10 mL of 1:1 water:THF and the mixture was cooled to 0° C. To the solution was added LiOH monohydrate (0.31 g, 7.4 mmol). The reaction mixture was allowed to come to room temperature. After stirring for 24 h, the reaction mixture was concentrated by in vacuo and the residue was dissolved in methylene chloride. The mixture was extracted 2×25 mL with water. The combined aqueous layers were neutralized with 1 N HCl to pH 4 and were extracted 2×25 mL with ethyl acetate. The combined ethyl acetate layers were dried over sodium sulfate and concentrated to give the title compound (360 mg, 83%) as yellow solid: MS (ESI, pos. ion) m/z 584 (M+H); HPLC (method B) tR=3.8 min, purity: >96%.

1. customto come to room temperature
2. concentrationthe reaction mixture was concentrated by in vacuo
3. dissolutionthe residue was dissolved in methylene chloride
4. extractionThe mixture was extracted 2×25 mL with water
5. extractionwere extracted 2×25 mL with ethyl acetate
6. dry with materialThe combined ethyl acetate layers were dried over sodium sulfate
7. concentrationconcentrated