HRID1508573

反应详情

EQUATION

反应方程式

HRID 1508573 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvent was removed
  2. additionwater was added
  3. additionA few drops of 1 N HCl were added
  4. extractionThe organic material was extracted with EtOAc (3×10 mL)
  5. dry with materialThe combined EtOAc layers were dried over Na2SO4
  6. customThe solvent was removed
  7. dissolutionThe residue was dissolved in CH2Cl2 (5 mL) at 25° C.
  8. washThe solution was washed with Na2S2O3
  9. dry with materialdried over Na2SO4
  10. customThe residue was purified by reverse phase HPLC