反应 #155383

ord-bce394fd86704cb8aed12f57cc631d5d

反应方程式

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

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08822042B2uspto-grants-2014_09