Reaktion #554616

ord-76e27b87190741a5b724e9b4411db060

Reaktionsgleichung

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

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeIn a reaction vessel equipped with an agitator
  2. 2
    Sonstigethe mixture was reacted at the same temperature for one hour
  3. 3
    Sonstigefurther reacted for one hour
  4. 4
    Extraktionextracted with ethyl acetate
  5. 5
    WaschenThe organic layer was washed with water
  6. 6
    Sonstigeseparated
  7. 7
    Trocknenit was then dried with magnesium sulfate
  8. 8
    Einengensubjected to vacuum concentration
  9. 9
    SonstigeThus, the objective product was obtained with the yield of 2.38 g

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08623577B2uspto-grants-2014_01