HRID1508573
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
A mixture of the title compound from Step C (150 mg, 0.216 mmol) and LiOH (51.8 mg, 2.16 mmol) was stirred in dioxane and water overnight. The solvent was removed and water was added. A few drops of 1 N HCl were added. The organic material was extracted with EtOAc (3×10 mL). The combined EtOAc layers were dried over Na2SO4. The solvent was removed. The residue was dissolved in CH2Cl2 (5 mL) at 25° C. and mCPBA (82 mg, 0.476 mmol) was added. The solution was stirred at 25° C. for 3 h. The solution was washed with Na2S2O3 and dried over Na2SO4. The residue was purified by reverse phase HPLC to give the title compound as a colorless solid. LCMS=712.6 (M+H)+
WORKUP
后处理
- customThe solvent was removed
- additionwater was added
- additionA few drops of 1 N HCl were added
- extractionThe organic material was extracted with EtOAc (3×10 mL)
- dry with materialThe combined EtOAc layers were dried over Na2SO4
- customThe solvent was removed
- dissolutionThe residue was dissolved in CH2Cl2 (5 mL) at 25° C.
- washThe solution was washed with Na2S2O3
- dry with materialdried over Na2SO4
- customThe residue was purified by reverse phase HPLC