تفاعل #955968

معادلة التفاعل

dichlorobenzene

(2-ethylhexyl)magnesium bromide

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product

المردود 21.0%

1,2-bis(2-ethylhexyl)benzene

المردود 21.0%

المذيبات

DI water

ظروف التفاعل

المعالجة

1. 1
   أخرىA dry 1 L three-neck round bottom flask, equipped with a condenser and an addition funnel
2. 2
   workup.ADDITIONAfter addition
3. 3
   درجة الحرارةthe reaction was heated
4. 4
   درجة الحرارةto reflux for 12 hours
5. 5
   درجة الحرارةcooled down to room temperature
6. 6
   استخلاصThe mixture was extracted with MTBE (3×100 mL)
7. 7
   تجفيفdried over anhydrous MgSO4
8. 8
   ترشيحfiltered
9. 9
   أخرىthe solvent was removed by rotary evaporation
10. 10
    workup.DISTILLATIONThe mixture was purified by distillation under a reduced pressure

الإجراء التجريبي

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.

المصدر