4,4'-[1,4-Phenylenebis(ethene-1,2-diyl)]bisbenzene synthesis
- Product Name:4,4'-[1,4-Phenylenebis(ethene-1,2-diyl)]bisbenzene
- CAS Number:1608-30-6
- Molecular formula:C22H18
- Molecular Weight:282.38
Yield:1608-30-6 96%
Reaction Conditions:
with bis(η3-allyl-μ-chloropalladium(II));6H-dibenzo[d,f-1,3]diazepin-6-ylidene-5,7-dihydro-5,7-diphenylphosphanyl;sodium carbonate in N,N-dimethyl acetamide at 130; for 48 h;Schlenk technique;Inert atmosphere;Heck Reaction;
Steps:
2.2 General procedure for the Heck coupling
General procedure: Na2CO3 (212 mg, 2 mmol), 4-chloronitrobenzene (1 mmol) and styrene (1.5 mmol) were added successively into a dried Schlenk tube under nitrogen. Then the DMA (0.1 mL) solution of DADPP (0.002 mmol) and [Pd(C3H5)Cl]2 (0.0005 mmol), which was reacted at 100 °C for 10 min prior to use, was added into the mixture. The reaction was performed at 130 °C. At the end of reaction, the mixture solution was extracted with ethyl acetate (3 × 5 mL). Combined organic phase was washed with brine (3 × 5 mL) and dried over MgSO4. The dried solution was filtered and purified with silica gel chromatography (petroleum ether 60-90 °C) to give a corresponding product.
References:
Jiang, Zhi-Jie;Wang, Wei;Zhou, Rong;Zhang, Lei;Fu, Hai-Yan;Zheng, Xue-Li;Chen, Hua;Li, Rui-Xiang [Catalysis Communications,2014,vol. 57,p. 14 - 18]
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