تفاعل #619275

معادلة التفاعل

diiodobiphenyl

carbazole

18-crown-6-ether

potassium carbonate

→

9-(4′-iodobiphenyl-4-yl)-9H-carbazole

المردود 89.0%

المذيبات

water

1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGAfter stirring
2. 2
   ترشيحthe mixture was filtrated
3. 3
   أخرىto give a precipitate
4. 4
   غسيلThe precipitate was washed with 1M hydrochloric acid, water
5. 5
   أخرىan aqueous solution of sodium hydrogen carbonate, and water in this order, and then was recrystallized from a mixture solution of toluene and hexane
6. 6
   أخرىThe resulting solid was recrystallized from chloroform

الإجراء التجريبي

Initially, 49 g (120 mmol) of diiodobiphenyl, 17 g (100 mmol) of carbazole, 1.0 g (5.0 mmol) of copper(I) iodide, 1.3 g (5.0 mmol) of 18-crown-6-ether, 10 g (75 mmol) of potassium carbonate, 40 mL of 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (abbreviation: DMPU) were put in a 500 mL three-neck flask, and the atmosphere of the flask was substituted by nitrogen. The mixture was stirred at 170° C. for 6.5 hours. After stirring, water was added to the mixture and the mixture was filtrated to give a precipitate. The precipitate was washed with 1M hydrochloric acid, water, an aqueous solution of sodium hydrogen carbonate, and water in this order, and then was recrystallized from a mixture solution of toluene and hexane. The resulting solid was recrystallized from chloroform to give 40 g of the target substance, white powder of 9-(4′-iodobiphenyl-4-yl)-9H-carbazole in a yield of 89%.

المصدر