反应 #502086

反应方程式

betulone aldehyde

H2O2

NaClO2

→

betulonic acid

溶剂

water

—

NaH2PO4.H2O

CH3CN—H2O

反应条件

后处理

1. 1
   温度the mixture warmed to room temperature
2. 2
   其他The reaction is quenched by addition of Na2S2O5 (380 mg)
3. 3
   萃取extracted with ethyl acetate
4. 4
   萃取The organic extract
5. 5
   洗涤is washed with water and brine
6. 6
   干燥dried (Na2SO4)
7. 7
   过滤filtered
8. 8
   浓缩concentrated

实验过程

The betulone aldehyde prepared from the last step is dissolved in a mixture of NaH2PO4.H2O (877 mg) and CH3CN—H2O (17 mL) and the suspension cooled to 0-5° C. 30% aqueous H2O2 (220 μL) and a solution of NaClO2 (200 mg) in water (16 mL) are then successively added, the mixture warmed to room temperature and stirred at this temperature for 1 h. The reaction is quenched by addition of Na2S2O5 (380 mg), and extracted with ethyl acetate. The organic extract is washed with water and brine, dried (Na2SO4), filtered, and concentrated. The residue is then subjected to column chromatography to afford betulonic acid (550 mg) as white solid.

来源