反应详情

The compound of Example 2 (0.7 g, 1.8 mmol), 4-fluorostyrene (1 g, 2.6 mmol), palladium acetate (0.03 g, 0.013 mmol) and tri-o-tolyphosphine (0.03 g, 0.01 mmol) were heated to 100°-120° C. in dimethylformamide (20 mL). After 3 h, palladium acetate (0.03 g, 0.013 mmol) was added and heating was continued for 2 h. The cooled reaction mixture was extracted with diethylether (50 mL) and water (100 mL). The diethylether solution was dried over magnesium sulfate and evaporated under reduced pressure. The residue was subjected to chromatography on silica gel using hexanes/ethyl acetate (6:1) as eluent. The product was isolated as a solid (0.28 g): m.p.: 154°-156° C. 1H NMR (CDCl3, 200 MHz) δ 7.5-7.0 (m,13H), 5.5 (m,1H), 4.8 (m,1H), 4.3 (m,1H).

1. temperatureheating
2. waitwas continued for 2 h
3. customThe cooled reaction mixture
4. extractionwas extracted with diethylether (50 mL) and water (100 mL)
5. dry with materialThe diethylether solution was dried over magnesium sulfate
6. customevaporated under reduced pressure