反应详情

Add n-butyl lithium solution (2.5 M, 140 mL, 350 mmol) to 3-bromoanisole (44.6 mL, 352.2 mmol) in cold (−78° C.) tetrahydrofuran (anhydrous, 500 mL), dropwise. Let stir for 10 minutes and add 2,4 difluorobenzaldehyde (50 g, 351 mmol), dropwise, and stir for an additional 1 hour. After 1 hour the reaction is complete. Quench the reaction mixture with cold water, extract with ethyl acetate, dry (MgSO4), and concentrate to give the crude, title compound (Compound 7) (90.21 g, >100% Yield). Use compound in a crude form or purify by column chromatography (20% ethyl acetate in heptane). NMR agrees with the final, desired compound.

1. stirringdropwise, and stir for an additional 1 hour
2. waitAfter 1 hour the reaction is complete
3. customQuench the reaction mixture with cold water
4. extractionextract with ethyl acetate
5. dry with materialdry (MgSO4)
6. concentrationconcentrate