반응 #577214

반응 방정식

m-chlorobenzoic acid

4-allyloxy-4′-cyanobiphenyl

→

4-cyano-4′-glycidylbiphenyl

수율 68.4%

용매

methylene chloride

반응 조건

후처리

1. 1
   기타obtained
2. 2
   기타Insoluble matters thus deposited were removed by filtration, and water
3. 3
   workup.ADDITIONwas added
4. 4
   기타After separating the mixture
5. 5
   세척the organic layer was washed with a saturated aqueous solution of sodium hydrosulfite
6. 6
   건조dried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONThe solvent was distilled off
8. 8
   기타to obtain a residue, which
9. 9
   기타was purified by silica gel column chromatography
10. 10
    기타subjected to recrystallization from ethanol

실험 절차

20 g of m-chlorobenzoic acid was added to a reaction mixture obtained by dissolving 19 g of 4-allyloxy-4′-cyanobiphenyl in 150 mL of methylene chloride as divided into several times, and the mixture was stirred at room temperature for 24 hours. Insoluble matters thus deposited were removed by filtration, and water was added thereto. After separating the mixture, the organic layer was washed with a saturated aqueous solution of sodium hydrosulfite and then dried over anhydrous magnesium sulfate. The solvent was distilled off to obtain a residue, which was purified by silica gel column chromatography and then subjected to recrystallization from ethanol to obtain 13 g of 4-cyano-4′-glycidylbiphenyl.

출처