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温度

0 °C

A dry 1 L three-neck round bottom flask, equipped with a condenser and an addition funnel, was charged with Ni(dppp)2Cl2 (0.99 g, 1.83 mmol) and dichlorobenzene (26.7 g, 182 mmol). The reaction solution was cooled down to 0° C. and then (2-ethylhexyl)magnesium bromide solution (400 mmol) was added dropwise via the addition funnel under nitrogen. After addition was complete, the reaction was heated to reflux for 12 hours and then cooled down to room temperature. The reaction solution was poured into 100 mL of DI water. The mixture was extracted with MTBE (3×100 mL). The organic phase was combined, dried over anhydrous MgSO4, filtered and the solvent was removed by rotary evaporation. The mixture was purified by distillation under a reduced pressure to give the product (11.5 g, 21%) as colorless oil.

1. customA dry 1 L three-neck round bottom flask, equipped with a condenser and an addition funnel
2. additionAfter addition
3. temperaturethe reaction was heated
4. temperatureto reflux for 12 hours
5. temperaturecooled down to room temperature
6. extractionThe mixture was extracted with MTBE (3×100 mL)
7. dry with materialdried over anhydrous MgSO4
8. filtrationfiltered
9. customthe solvent was removed by rotary evaporation
10. distillationThe mixture was purified by distillation under a reduced pressure