반응 #497187

반응 방정식

n-BuLi

4-bromobiphenyl

SnBu3Cl

→

4-tributylstannylbiphenyl

반응 조건

후처리

1. 1
   기타reacted at −78° C. for 40 minutes under
2. 2
   기타a dry
3. 3
   기타anaerobic operation condition to form a solution
4. 4
   기타reacted at −78° C. for 1 hour
5. 5
   기타After returning to room temperature
6. 6
   기타the solution was continuously reacted for 8 hours
7. 7
   추출the solution was extracted by ether (30 mL) and deionized water (50 mL)
8. 8
   기타An organic phase was collected
9. 9
   기타After removal of ether by a rotary concentrator
10. 10
    workup.DISTILLATIONthe organic phase was purified by reduced-pressure distillation
11. 11
    기타to form a transparent colorless oily product (21, 1.83 g, 78%)

실험 절차

2.5 M of n-BuLi (2.1 mL/hexane, 5.32 mmol) was added to 4-bromobiphenyl (1.24 g, 5.32 mmol/THF (20 mL)) and reacted at −78° C. for 40 minutes under a dry and anaerobic operation condition to form a solution. SnBu3Cl (1.65 mL, 5.85 mmol) was then added to the solution and reacted at −78° C. for 1 hour. After returning to room temperature, the solution was continuously reacted for 8 hours. After the reaction was completed, the solution was extracted by ether (30 mL) and deionized water (50 mL). An organic phase was collected. After removal of ether by a rotary concentrator, the organic phase was purified by reduced-pressure distillation to form a transparent colorless oily product (21, 1.83 g, 78%).

출처