تفاعل #577214

معادلة التفاعل

m-chlorobenzoic acid

4-allyloxy-4′-cyanobiphenyl

→

4-cyano-4′-glycidylbiphenyl

المردود 68.4%

المذيبات

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   أخرىobtained
2. 2
   أخرىInsoluble matters thus deposited were removed by filtration, and water
3. 3
   workup.ADDITIONwas added
4. 4
   أخرىAfter separating the mixture
5. 5
   غسيلthe organic layer was washed with a saturated aqueous solution of sodium hydrosulfite
6. 6
   تجفيفdried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONThe solvent was distilled off
8. 8
   أخرىto obtain a residue, which
9. 9
   أخرىwas purified by silica gel column chromatography
10. 10
    أخرىsubjected to recrystallization from ethanol

الإجراء التجريبي

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.

المصدر