HRID865530
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationThe reaction mixture was then filtered through a bed of celite and MgSO4
- customthe flitrate was evaporated in vacuo
- dissolutionThe residue was dissolved in dichloromethane
- washeluted with 3% MeOH
- customEvaporation of the purified fractions
- customdrying in vacuo