반응 #2122466

반응 방정식

4,4′-bis(chloromethyl)-1,1′-biphenyl

p-xylene

→

4,4′-bis(2,5-dimethylbenzyl)-1,1′-biphenyl

용매

ethanol

반응 조건

후처리

1. 1
   workup.STIRRINGAfter stirring overnight at room temperature
2. 2
   기타The mixture was transferred to a separatory funnel
3. 3
   세척washed with dilute aqueous HCl
4. 4
   건조The organic layer was dried over magnesium sulfate
5. 5
   농축concentrated to dryness under vacuum on a rotary evaporator
6. 6
   기타The tan solid was recrystallized from toluene yielding a white crystalline product, mp=144.6 C

실험 절차

A 100mL flask was charged with 4,4′-bis(chloromethyl)-1,1′-biphenyl (1.0 g) and p-xylene (25 mL). To the clear solution stirring at room temperature was added titanium tetrachloride (6 drops) and the mixture instantly became dark brown. After stirring overnight at room temperature, ethanol (2mL) was added to kill the catalyst, and the mixture became a light, cream colored suspension. The mixture was transferred to a separatory funnel and washed with dilute aqueous HCl followed by saturated aqueous sodium bicarbonate. The organic layer was dried over magnesium sulfate, and concentrated to dryness under vacuum on a rotary evaporator. The tan solid was recrystallized from toluene yielding a white crystalline product, mp=144.6 C. GC/MS, HNMR, CNMR and IR were all consistent with the desired product.

출처