Hexane → HCID 178506790, Verbindung

A solution of fresh LiC≡CPh was prepared by reacting 0.057 mL of phenylacetylene (0.525 mmol) and 0.298 mL of 1.5M nBuLi in hexane solution (0.462 mmol) in 15 mL of dry THF at −78° C. for 0.5 hour. The resulting solution was added drop wise via cannula to a solution of 160 mg of Ir(ppy)2(CNtBu)OTf (0.22 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 and the crude was extracted with diethylether. 67.8 mg of Ir(ppy)2(CNtBu)(CCPh) is obtained (45% yield).

1. customat −78° C.
2. customfor 0.5 hour
3. customThe mixture was reacted for 1 h at −78° C.
4. customThe solvent was removed under reduced pressure
5. extractionthe crude was extracted with diethylether

ORD-Eintrag

ord-8d12691b227548f1baa85a9b80aede5b

Quelldatensatz

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08822042B2