Reacción #955968

Ecuación de reacción

dichlorobenzene

(2-ethylhexyl)magnesium bromide

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product

Rendimiento 21.0%

1,2-bis(2-ethylhexyl)benzene

Rendimiento 21.0%

Disolventes

DI water

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroA dry 1 L three-neck round bottom flask, equipped with a condenser and an addition funnel
2. 2
   workup.ADDITIONAfter addition
3. 3
   Temperaturathe reaction was heated
4. 4
   Temperaturato reflux for 12 hours
5. 5
   Temperaturacooled down to room temperature
6. 6
   ExtracciónThe mixture was extracted with MTBE (3×100 mL)
7. 7
   Secadodried over anhydrous MgSO4
8. 8
   Filtraciónfiltered
9. 9
   Otrothe solvent was removed by rotary evaporation
10. 10
    workup.DISTILLATIONThe mixture was purified by distillation under a reduced pressure

Procedimiento

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.

Fuente