反应 #554616

ord-76e27b87190741a5b724e9b4411db060

反应方程式

BrB(Br)Br
boron tribromide
COc1ccc2cc(N(c3ccc(C)cc3)c3ccc4cc(OC)ccc4c3)ccc2c1
p-tolyl-bis(6-methoxy-2-naphthyl)amine
Cc1ccc(N(c2ccc3cc(O)ccc3c2)c2ccc3cc(O)ccc3c2)cc1
p-tolyl-bis(6-hydroxy-2-naphthyl)amine

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他In a reaction vessel equipped with an agitator
  2. 2
    其他the mixture was reacted at the same temperature for one hour
  3. 3
    其他further reacted for one hour
  4. 4
    萃取extracted with ethyl acetate
  5. 5
    洗涤The organic layer was washed with water
  6. 6
    其他separated
  7. 7
    干燥it was then dried with magnesium sulfate
  8. 8
    浓缩subjected to vacuum concentration
  9. 9
    其他Thus, the objective product was obtained with the yield of 2.38 g

实验过程

In a reaction vessel equipped with an agitator, thermometer and a cooling pipe, 2.1 g of p-tolyl-bis(6-methoxy-2-naphthyl)amine and 50 mL of methylene chloride were placed. While the vessel was being cooled with ice, 12 mL of a 1M methylene chloride solution of boron tribromide was delivered by drops into the vessel, and the mixture was reacted at the same temperature for one hour. The temperature was raised to a room temperature and further reacted for one hour. Then, the reacted solution was poured into ice water and extracted with ethyl acetate. The organic layer was washed with water and separated, and it was then dried with magnesium sulfate and subjected to vacuum concentration. Thus, the objective product was obtained with the yield of 2.38 g.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08623577B2uspto-grants-2014_01