反应 #2122466

反应方程式

4,4′-bis(chloromethyl)-1,1′-biphenyl

p-xylene

→

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

溶剂

ethanol

反应条件

后处理

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

实验过程

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.

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