반응 #502084

반응 방정식

Betulin

Jones Reagent

→

betulonic acid

용매

benzene

methanol

acetone

반응 조건

후처리

1. 1
   workup.ADDITIONadded dropwise at 0° C
2. 2
   기타quench with methanol (100 mL)
3. 3
   workup.STIRRINGstir for 5 minutes
4. 4
   workup.ADDITIONadd H2O (200 mL)
5. 5
   기타Remove organic solvent under vacuum, and then separate the precipitate
6. 6
   여과by filtration
7. 7
   세척Wash precipitate on the
8. 8
   여과filter with cooled water
9. 9
   기타dry
10. 10
    기타to obtain crude material
11. 11
    여과The 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
    기타The precipitate is then separated by filtration
14. 14
    세척washed with 10 mL
15. 15
    온도cooled benzene
16. 16
    기타dried
17. 17
    기타to obtain white solid
18. 18
    workup.ADDITIONthe solution is poured into 100 mL 15% aqueous HCL solution

실험 절차

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.

출처