Реакция #155382

Уравнение реакции

hexane

phenylacetylene

nBuLi

→

LiC≡CPh

Выход 45.0%

Растворители

THF

THF

Условия реакции

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
5. 5
   Экстракцияthe crude was extracted with diethylether

Методика

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).

Источник