반응 #2069930

반응 방정식

m-chloroperbenzoic acid

4-allyloxy-4′-cyanobiphenyl

→

4-cyano-4′-glycidylbiphenyl

수율 68.4%

용매

methylene chloride

반응 조건

후처리

1. 1
   workup.ADDITIONwas added in a few times to a solution
2. 2
   기타prepared
3. 3
   여과The deposited insoluble was filtered away
4. 4
   workup.ADDITIONwater was added to it for liquid-liquid separation
5. 5
   세척the organic layer was washed with an aqueous saturated sodium hydrosulfite solution
6. 6
   건조dried with anhydrous magnesium sulfate
7. 7
   기타The solvent was evaporated away
8. 8
   기타the residue was purified through silica gel column chromatography
9. 9
   기타further recrystallized from ethanol

실험 절차

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.

출처