تفاعل #502084

معادلة التفاعل

Betulin

Jones Reagent

→

betulonic acid

المذيبات

benzene

methanol

acetone

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONadded dropwise at 0° C
2. 2
   أخرىquench with methanol (100 mL)
3. 3
   workup.STIRRINGstir for 5 minutes
4. 4
   workup.ADDITIONadd H2O (200 mL)
5. 5
   أخرىRemove organic solvent under vacuum, and then separate the precipitate
6. 6
   ترشيحby filtration
7. 7
   غسيلWash precipitate on the
8. 8
   ترشيحfilter with cooled water
9. 9
   أخرىdry
10. 10
    أخرىto obtain crude material
11. 11
    ترشيحThe 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
    أخرىThe precipitate is then separated by filtration
14. 14
    غسيلwashed with 10 mL
15. 15
    درجة الحرارةcooled benzene
16. 16
    أخرىdried
17. 17
    أخرىto obtain white solid
18. 18
    workup.ADDITIONthe solution is poured into 100 mL 15% aqueous HCL solution

الإجراء التجريبي

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.

المصدر