Реакция #554616

ord-76e27b87190741a5b724e9b4411db060

Уравнение реакции

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

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеIn a reaction vessel equipped with an agitator
  2. 2
    Другоеthe mixture was reacted at the same temperature for one hour
  3. 3
    Другоеfurther reacted for one hour
  4. 4
    Экстракцияextracted with ethyl acetate
  5. 5
    ПромывкаThe organic layer was washed with water
  6. 6
    Другоеseparated
  7. 7
    Сушкаit was then dried with magnesium sulfate
  8. 8
    Концентрированиеsubjected to vacuum concentration
  9. 9
    ДругоеThus, the objective product was obtained with the yield of 2.38 g

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08623577B2uspto-grants-2014_01