반응 #6418

반응 방정식

toluene

p-(7-octenyloxy)benzoic acid

toluene

2-methylbutyl 4'-hydroxybiphenyl-4-carboxylate

Toluene

toluene

p-(7-octenyloxy)benzoic acid

→

ester

수율 45.0%

2-methylbutyl 4-[p-(7-octenyloxy)benzoyloxy]biphenyl-4-carboxylate

수율 45.0%

용매

pyridine

반응 조건

후처리

1. 1
   온도the temperature was raised
2. 2
   기타reaction
3. 3
   기타After conclusion of the reaction
4. 4
   세척the product was washed with water
5. 5
   건조dried over magnesium sulfate
6. 6
   농축concentrated under reduced pressure
7. 7
   기타The residue was recrystallized from ethanol

실험 절차

9 g of p-(7-octenyloxy)benzoic acid obtained in 15.(1) was suspended in toluene, and the suspension was cooled in an ice bath. Added dropwise thereto was 6 g of thionyl chloride. After conclusion of the dropping, the temperature was raised and reaction was carried out for 6 hours at 80° C. After conclusion of the reaction, the reaction solution was concentrated under reduced pressure, to obtain an acid chloride compound. Toluene was added to the acid chloride compound, and the resulting toluene solution was cooled in an ice bath. A toluene solution containing 10 g of 2-methylbutyl 4'-hydroxybiphenyl-4-carboxylate and 3 g of pyridine was added dropwise into the above-described toluene solution of the acid chloride compound. After conclusion of dropping, the temperature was raised, and reaction was carried out for 8 hours at 50° C. After conclusion of the reaction, the product was washed with water, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was recrystallized from ethanol, to obtain 8.2 g of the objective ester compound. (Yield: 45%)

출처