反応 #2069930

反応方程式

m-chloroperbenzoic acid

4-allyloxy-4′-cyanobiphenyl

→

4-cyano-4′-glycidylbiphenyl

収率 68.4%

溶媒

methylene chloride

反応条件

後処理

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

実験手順

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.

出典