反应详情

温度

5 °C

A dry 2 L 3-neck flask with attached reflux condenser and addition funnel, flushed with dry nitrogen, was charged with 1,2-dichlorobenzene (79.4 g, 540 mmol), Ni(dppp)Cl2 (3 g, 6 mmol), and 200 mL of dry Et2O. The addition funnel was charged with 2-ethylhexylmagnesium bromide (3M, 400 mL). The solution was cooled to 5° C. and the Grignard reagent was added dropwise to the reaction. After complete addition, the reaction was stirred at 5° C. for 30 min and then warmed to room temperature (RT). The reaction was then heated to reflux for 12 h. After cooling to RT, the reaction mixture was poured onto an ice/HCl (10%) solution and extracted with MTBE. The organic fractions were dried over anhydrous MgSO4 and then concentrated. The product was purified first by distillation followed by column chromatography with hexanes, and isolated as colorless oil (101 g, 62%).

1. temperatureA dry 2 L 3-neck flask with attached reflux
2. additioncondenser and addition funnel
3. customflushed with dry nitrogen
4. additionAfter complete addition
5. temperaturewarmed to room temperature (RT)
6. temperatureThe reaction was then heated
7. temperatureto reflux for 12 h
8. temperatureAfter cooling to RT
9. extractionextracted with MTBE
10. dry with materialThe organic fractions were dried over anhydrous MgSO4
11. concentrationconcentrated
12. distillationThe product was purified first by distillation