HRID254257
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
4.69 mL (23.55 mmol, 1 eq.) of 3,3-diphenylpropanol are dissolved in 100 mL of CH2Cl2 under argon. 10.5 g (24.73 mmol, 1.05 eq.) of Dess Martin Periodinane (1,1,1-triacetoxy-1,1-dihydro-1,2-benziodoxol-3(1H)-one) are added to the mixture and the solution is stirred for 1 hour 30 min at 0° C. 100 mL of 2 M sodium hydroxide and 100 mL of CH2Cl2 are then added. The organic phase is washed with 2 M sodium hydroxide (twice), with water (twice), dried over MgSO4, filtered and concentrated. The crude reaction product is subjected to chromatography over silica gel (eluent: 5/1 heptane/AcOEt). An oil which crystallises in the form of a white product is recovered (4.76 g, yield=96%).
WORKUP
后处理
- washThe organic phase is washed with 2 M sodium hydroxide (twice), with water (twice),
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customThe crude reaction product
- customAn oil which crystallises in the form of a white product
- customis recovered (4.76 g, yield=96%)