반응 #1884058

반응 방정식

n-butyl lithium

dibromothiophene

trimethylstannyl chloride

→

title compound

수율 61.0%

2,5-bis(trimethylstannyl)thiophene

수율 61.0%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.WAITthe reaction was continued at −50° C. for about 4˜5 hours
2. 2
   기타Next, the aqueous layer and organic layer were separated
3. 3
   기타The obtained organic layer was dried over a drying agent
4. 4
   기타solvents were removed
5. 5
   기타The resulting crude product was recrystallized from ether twice

실험 절차

After 18.4 mL (30 mmol) of n-butyl lithium solution (n-BuLi, 1.63M in hexane) was added to a solution of 3.0 g (12.4 mmol) dibromothiophene in tetrahydrofuran (50 mL) at −50° C. under nitrogen atmosphere, the reaction was allowed to proceed for 30 minutes. To the mixture was added 5 g of trimethylstannyl chloride (SnMe3Cl, 25 mmol) and the reaction was continued at −50° C. for about 4˜5 hours. Next, the aqueous layer and organic layer were separated. The obtained organic layer was dried over a drying agent, and then solvents were removed. The resulting crude product was recrystallized from ether twice to afford 3.1 g (yield: 60%) of the title compound as a white crystal.

출처