تفاعل #689399

معادلة التفاعل

potassium hydroxide

N-(4′-iodobiphenylyl)acetanilide

potassium carbonate

n-dodecane

→

N-(4-biphenylyl)-N,N′-diphenyl-4,4′-diaminobiphenyl

المردود 77.8%

المذيبات

water

isoamyl alcohol

ظروف التفاعل

المعالجة

1. 1
   أخرىfollowed by reaction at 200 to 212° C. for 15 hours
2. 2
   استخلاصThe reaction product was extracted with 200 ml of toluene
3. 3
   أخرىthe insoluble matter was removed by filtration
4. 4
   تركيزThen, the filtrate was concentrated
5. 5
   أخرىto obtain oily matter
6. 6
   أخرىfollowed by hydrolysis at 130° C
7. 7
   أخرىAfter isoamyl alcohol was removed by steam distillation, extraction with 250 ml of toluene
8. 8
   غسيلby washing with water
9. 9
   أخرىdrying
10. 10
    تركيزconcentration
11. 11
    أخرىThe concentrate was purified by column chromatography (carrier: silica gel, eluate: toluene/n-hexane=1/2)

الإجراء التجريبي

There were mixed 16.5 g (0.040 mole) of N-(4′-iodobiphenylyl)acetanilide, 11.8 g (0.048 mole) of N-(4-biphenyl)aniline, 8.3 g (0.060 mole) of anhydrous potassium carbonate, 0.1 g (0.002 mole) of copper powder and 10 ml of n-dodecane, followed by reaction at 200 to 212° C. for 15 hours. The reaction product was extracted with 200 ml of toluene, and the insoluble matter was removed by filtration. Then, the filtrate was concentrated to obtain oily matter. The oily matter was dissolved in 60 ml of isoamyl alcohol, and 4 ml of water and 4.00 g (0.060 mole) of 85% potassium hydroxide were added, followed by hydrolysis at 130° C. After isoamyl alcohol was removed by steam distillation, extraction with 250 ml of toluene was performed, followed by washing with water, drying and concentration. The concentrate was purified by column chromatography (carrier: silica gel, eluate: toluene/n-hexane=1/2) to obtain 15.2 g (yield: 77.8%, HPLC purity: 97.0%) of N-(4-biphenylyl)-N,N′-diphenyl-4,4′-diaminobiphenyl. The melting point was 126.6 to 127.4° C.

المصدر