HRID865530

反应详情

EQUATION

反应方程式

HRID 865530 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 0.573 g (1.09 mmol) of the product of Example 65 dissolved in 5.0 mL of dichloromethane was added 2.86 g (32.9 mmol) of manganese dioxide and 1.15 g of finely powdered 3A molecular sieves and the reaction mixture was magnetically stirred at room temperature for 14 hours. The reaction mixture was then filtered through a bed of celite and MgSO4 and the flitrate was evaporated in vacuo. The residue was dissolved in dichloromethane and applied to a silica gel flash chromatography column and then eluted with 3% MeOH--CH2Cl2. Evaporation of the purified fractions and drying in vacuo afforded 0.149 g (26%) of the title compound.

WORKUP

后处理

  1. filtrationThe reaction mixture was then filtered through a bed of celite and MgSO4
  2. customthe flitrate was evaporated in vacuo
  3. dissolutionThe residue was dissolved in dichloromethane
  4. washeluted with 3% MeOH
  5. customEvaporation of the purified fractions
  6. customdrying in vacuo