反应详情

温度

-78 °C

To a solution of 4′-chloro-4-biphenylcarbaldehyde (200 mg, 0.92 mmol) in anhydrous THF (10 mL) under nitrogen at −78° C. (dry ice/acetone) was added nBuMgCl (550 μL of a 2M solution in THF, 1.10 mmol). The reaction mixture was stirred at −78° C. for 1 hour and then at rt for 18 hours. The reaction was quenched by cautious addition of water (15 mL) and extracted with EtOAc (3×20 mL). The combined organic extract was then dried (MgSO4) and reduced under vacuum. Purification by flash chromatography (silica), eluting with cyclohexane:EtOAc (9:1) afforded the title compound as a colourless gum (140 mg).

1. waitat rt for 18 hours
2. customThe reaction was quenched by cautious addition of water (15 mL)
3. extractionextracted with EtOAc (3×20 mL)
4. extractionThe combined organic extract
5. dry with materialwas then dried (MgSO4)
6. customPurification by flash chromatography (silica)
7. washeluting with cyclohexane:EtOAc (9:1)