反应详情

温度

0 °C

To a solution of 3-chlorothiophene (384 mg, 3.0 mmol) in THF (6 mL) at −78° C. was added n-BuLi (1.6 M, 2 mL) and the resulting mixture stirred for 45 minutes. The resulting product was added to a solution of 2,4-dichloropyrimidine (430 mg, 2.9 mmol) in ether (10 mL) at −30° C. and the resulting mixture stirred for 30 minutes, then warmed up to 0° C. and stirred for another 30 minutes. DDQ (700 mg, 3 mmol) was added and the resulting mixture was stirred overnight, then filtered through Celite®. The filtrate was concentrated and the residue was purified by silica gel column (EtOAc/hexanes, 1:5) to yield a white solid.

1. stirringthe resulting mixture stirred for 30 minutes
2. stirringstirred for another 30 minutes
3. stirringthe resulting mixture was stirred overnight
4. filtrationfiltered through Celite®
5. concentrationThe filtrate was concentrated
6. customthe residue was purified by silica gel column (EtOAc/hexanes, 1:5)
7. customto yield a white solid