反応 #155382

反応方程式

hexane

phenylacetylene

nBuLi

→

LiC≡CPh

収率 45.0%

溶媒

THF

THF

反応条件

後処理

1. 1
   その他at −78° C.
2. 2
   その他for 0.5 hour
3. 3
   その他The mixture was reacted for 1 h at −78° C.
4. 4
   その他The solvent was removed under reduced pressure
5. 5
   抽出the crude was extracted with diethylether

実験手順

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).

出典