HRID1466733

反应详情

EQUATION

反应方程式

HRID 1466733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 24 (488.2 mg, 1.5 mmol) in 12 mL of dry CH2Cl2 at 0° C. was added a solution of MCPBA (403.4 mg, 1.80 mmol in 4 mL of CH2Cl2), the reaction mixture was stirred at 0° C. for 1 hr and then quenched with saturated aqueous NaHCO3 (50 mL). Et2O (3×50 mL) was then added, and the organic layer was washed with saturated aqueous NaHCO3, water, and brine, and dried with MgSO4 and concentrated to give a crude product. The crude product was passed through a silica gel column (hexanes/EtOAc 80:1, 40:1, 20:1) to give the pure epoxide 25 (104 mg: yield 20%) as a colorless oil.

WORKUP

后处理

  1. customquenched with saturated aqueous NaHCO3 (50 mL)
  2. additionEt2O (3×50 mL) was then added
  3. washthe organic layer was washed with saturated aqueous NaHCO3, water, and brine
  4. dry with materialdried with MgSO4
  5. concentrationconcentrated
  6. customto give a crude product