反应 #554615

反应方程式

boron tribromide

N,N-di-p-tolyl-N′,N′-bis(4′-methoxybiphenyl-4-yl)benzidine

→

N,N-di-p-tolyl-N′,N′-bis(4′-hydroxybiphenyl-4-yl)benzidine

溶剂

methylene chloride

methylene chloride

反应条件

后处理

1. 1
   其他In a reaction vessel equipped with an agitator
2. 2
   其他was reacted at the same temperature for three hours
3. 3
   萃取extracted with methylene chloride
4. 4
   洗涤The organic layer was washed with water
5. 5
   其他separated
6. 6
   干燥it was then dried with magnesium sulfate
7. 7
   浓缩subjected to vacuum concentration
8. 8
   其他The residue was purified with a silica gel chromatography with a mixture of n-hexane and ethyl acetate as a solvent
9. 9
   其他Thus, the objective product was obtained with the yield of 2.53 g

实验过程

In a reaction vessel equipped with an agitator, thermometer and a cooling pipe, 2.73 g of N,N-di-p-tolyl-N′,N′-bis(4′-methoxybiphenyl-4-yl)benzidine and 100 mL of methylene chloride were placed. While the vessel was being cooled with ice, 10 mL of a 1M methylene chloride solution of boron tribromide was delivered by drops into the vessel, and furthermore the mixture was reacted at the same temperature for three hours. Then, the reacted solution was poured into ice water and extracted with methylene chloride. The organic layer was washed with water and separated, and it was then dried with magnesium sulfate and subjected to vacuum concentration. The residue was purified with a silica gel chromatography with a mixture of n-hexane and ethyl acetate as a solvent, where the ratio of n-hexane to ethyl acetate in the mixture was one to one. Thus, the objective product was obtained with the yield of 2.53 g.

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