반응 #955968

반응 방정식

dichlorobenzene

(2-ethylhexyl)magnesium bromide

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product

수율 21.0%

1,2-bis(2-ethylhexyl)benzene

수율 21.0%

용매

DI water

반응 조건

후처리

1. 1
   기타A dry 1 L three-neck round bottom flask, equipped with a condenser and an addition funnel
2. 2
   workup.ADDITIONAfter addition
3. 3
   온도the reaction was heated
4. 4
   온도to reflux for 12 hours
5. 5
   온도cooled down to room temperature
6. 6
   추출The mixture was extracted with MTBE (3×100 mL)
7. 7
   건조dried over anhydrous MgSO4
8. 8
   여과filtered
9. 9
   기타the solvent was removed by rotary evaporation
10. 10
    workup.DISTILLATIONThe mixture was purified by distillation under a reduced pressure

실험 절차

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.

출처