反应详情

温度

50 °C

A suspension consisting of 1,1′-(4-bromobutylidene)bis[4-fluorobenzene] (25 g, 77 mmol) and potassium phthalimide (17 g, 92 mmol) in 300 mL DMF was stirred at 50° C. for 16 hours, cooled to 25° C., and poured into 900 mL of cold H2O. The mixture was extracted with ethyl acetate (3×300 mL), and the combined extracts were washed with H2O (2×1 L), followed by brine (700 mL), then dried over anhydrous sodium sulfate. Evaporation of solvent in vacuo afforded 28.6 g of a golden oil, which was triturated with 250 mL 2,2,4-trimethylpentane containing 5% 2-propanol, and the solid thus obtained was collected by filtration and dried at 50° C. in vacuo, to give 28.7 g (97%) of titled compound as a white powder; mp 69-70° C. APCI-MS m/z 391.1 (M−).

1. temperaturecooled to 25° C.
2. extractionThe mixture was extracted with ethyl acetate (3×300 mL)
3. washthe combined extracts were washed with H2O (2×1 L)
4. dry with materialdried over anhydrous sodium sulfate
5. customEvaporation of solvent in vacuo