Reaction equation
[C:1]1([C:7]#[CH:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CCCCCC.[Li:15]CCCC>C1COCC1>[Li:15][C:8]#[C:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
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.
Workup
- customat −78° C.
- customfor 0.5 hour
- customThe mixture was reacted for 1 h at −78° C.
- customThe solvent was removed under reduced pressure
Sources & evidence
- ORD record
- ord-bce394fd86704cb8aed12f57cc631d5d
- Source dataset
- uspto-grants-2014_09
- Patent number
- US08822042B2
Linked notes
Loading…