反应 #502084

反应方程式

Betulin

Jones Reagent

→

betulonic acid

溶剂

benzene

methanol

acetone

反应条件

后处理

1. 1
   workup.ADDITIONadded dropwise at 0° C
2. 2
   其他quench with methanol (100 mL)
3. 3
   workup.STIRRINGstir for 5 minutes
4. 4
   workup.ADDITIONadd H2O (200 mL)
5. 5
   其他Remove organic solvent under vacuum, and then separate the precipitate
6. 6
   过滤by filtration
7. 7
   洗涤Wash precipitate on the
8. 8
   过滤filter with cooled water
9. 9
   其他dry
10. 10
    其他to obtain crude material
11. 11
    过滤The solution is then filtered through a layer of aluminum oxide
12. 12
    workup.ADDITIONthe eluate is treated with an aqueous 10% KOH solution until complete precipitation
13. 13
    其他The precipitate is then separated by filtration
14. 14
    洗涤washed with 10 mL
15. 15
    温度cooled benzene
16. 16
    其他dried
17. 17
    其他to obtain white solid
18. 18
    workup.ADDITIONthe solution is poured into 100 mL 15% aqueous HCL solution

实验过程

Starting off with Betulin (10 g) in acetone (300 mL), add freshly prepared Jones Reagent added dropwise at 0° C. Stir for 5 hours, quench with methanol (100 mL), then stir for 5 minutes and add H2O (200 mL). Remove organic solvent under vacuum, and then separate the precipitate by filtration. Wash precipitate on the filter with cooled water, and dry to obtain crude material. This dry material is to be dissolved in 30 mL benzene. The solution is then filtered through a layer of aluminum oxide and the eluate is treated with an aqueous 10% KOH solution until complete precipitation. The precipitate is then separated by filtration, washed with 10 mL cooled benzene, and dried to obtain white solid. The salt is dissolved in 30 mL methanol and the solution is poured into 100 mL 15% aqueous HCL solution. The betulonic acid (2.7 g) is obtained after the precipitate is filtered, washed with water, and dried.

来源