Реакция #155383

ord-bce394fd86704cb8aed12f57cc631d5d

Уравнение реакции

C#Cc1ccccc1
phenylacetylene
CCCCCC.[Li][CH2]CCC
hexane nBuLi
[Li][C]#Cc1ccccc1
LiC≡CPh

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеat −78° C.
  2. 2
    Другоеfor 0.5 hour
  3. 3
    ДругоеThe mixture was reacted for 1 h at −78° C.
  4. 4
    ДругоеThe solvent was removed under reduced pressure

Методика

A solution of fresh LiC≡CPh was prepared by reacting 0.118 mL of phenylacetylene (1.08 mmol) and 0.48 mL of 1.5M hexane nBuLi solution (0.72 mmol) in 50 mL of dry THF at −78° C. for 0.5 hour. The solution was added drop wise via cannula to a solution of 150 mg of Ir(ppy)2(MeOH)2OTf (0.18 mmol) in 10 mL of dry THF at −78° C. The mixture was reacted for 1 h at −78° C. and the temperature was raised to RT over 2 hours. The solvent was removed under reduced pressure obtaining the Ir(ppy)2(CCPh)2Li.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08822042B2uspto-grants-2014_09