反应 #1544082

反应方程式

digoxigenin

cyclohexanone

aluminum isopropoxide

→

white solid

收率 189.5%

3-Ketodigoxigenin

收率 189.5%

溶剂

toluene

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度under reflux for 2.3 hours
3. 3
   浓缩concentrated in vacuo to half of its original volume
4. 4
   workup.ADDITIONTwo hundred μl water was added
5. 5
   其他the mixture was evaporated in vacuo to dryness
6. 6
   其他The powdery solid was dried in vacuo over overnight
7. 7
   过滤the resulting mixture was filtered
8. 8
   洗涤The residue on the funnel was washed with 25 ml methanol
9. 9
   洗涤The filtrate and washing
10. 10
    其他evaporated in vacuo

实验过程

A mixture of 488 mg digoxigenin, 7.5 ml toluene, 3.75 ml cyclohexanone, and 550 mg aluminum isopropoxide was heated under reflux for 2.3 hours and then concentrated in vacuo to half of its original volume. Two hundred μl water was added and the mixture was evaporated in vacuo to dryness. The powdery solid was dried in vacuo over overnight. The dry residue was stirred in 25 ml methanol and the resulting mixture was filtered. The residue on the funnel was washed with 25 ml methanol. The filtrate and washing were combined and evaporated in vacuo affording 920 mg white solid.

来源