反应 #2069930

反应方程式

m-chloroperbenzoic acid

4-allyloxy-4′-cyanobiphenyl

→

4-cyano-4′-glycidylbiphenyl

收率 68.4%

溶剂

methylene chloride

反应条件

后处理

1. 1
   workup.ADDITIONwas added in a few times to a solution
2. 2
   其他prepared
3. 3
   过滤The deposited insoluble was filtered away
4. 4
   workup.ADDITIONwater was added to it for liquid-liquid separation
5. 5
   洗涤the organic layer was washed with an aqueous saturated sodium hydrosulfite solution
6. 6
   干燥dried with anhydrous magnesium sulfate
7. 7
   其他The solvent was evaporated away
8. 8
   其他the residue was purified through silica gel column chromatography
9. 9
   其他further recrystallized from ethanol

实验过程

20 g of m-chloroperbenzoic acid divided into portions was added in a few times to a solution prepared by dissolving 19 g of 4-allyloxy-4′-cyanobiphenyl in 150 ml of methylene chloride, and stirred at room temperature for 24 hours. The deposited insoluble was filtered away, water was added to it for liquid-liquid separation, and the organic layer was washed with an aqueous saturated sodium hydrosulfite solution and then dried with anhydrous magnesium sulfate. The solvent was evaporated away, and the residue was purified through silica gel column chromatography and further recrystallized from ethanol to obtain 13 g of 4-cyano-4′-glycidylbiphenyl.

来源