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张超峰

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The influence of various organic and inorganic bases such as K3PO4, Cs2CO3, KOtBu, K2CO3 and KOH was studied for the standard reaction (entries 1, 5–8). It was observed that the bases K2CO3, Cs2CO3 and K3PO4 a or-ded good yields of the desired product. However, due to cost considerations K3PO4 was preferred over Cs2CO3. The e ect of various solvents on the reaction system was also examined (entries 1, 9–12). It was observed that non-polar solvents such as toluene gave a low yield of product probably due to the poor solubility of reactant and catalyst in the reaction medium. It was also observed that pro-longed reaction of the catalyst in toluene led to decompo-sition of the catalyst and precipitation of Pd metal. The use of polar solvents such as NMP and DMSO led to an increase in the yield without any catalyst deactivation. However, N-methyl-2-pyrrolidine (NMP) was found to give the best results and was used for further studies.
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cfk580713

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sltmac: 金币+1 2012-05-08 08:54:55
张超峰: 金币+20, 翻译EPI+1 2012-05-08 09:23:13
研究了大量有机和无机碱,如 K3PO4, Cs2CO3, KOtBu, K2CO3 和 KOH 对标准反应的影响。结果表明,在 K2CO3, Cs2CO3和K3PO4作用下都能以较高产率得到目标产物。 然而,基于成本考虑,我们更倾向于使用K3PO4,而不是Cs2CO3. 同时,也研究了不同溶剂对反应体系的影响(entries 1, 9–12). 结果表明,在如甲苯等非极性溶剂中反应的产率较低,其原因可能是在非极性反应介质中,反应物及催化剂地溶解性不好.
2楼2012-05-07 22:08:58
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cfk580713

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张超峰: 金币+10 2012-05-08 09:23:19
同时,我们也发现延长催化剂在甲苯中的反应时间会导致催化剂的分解以及Pd金属沉淀。而使用NMP,DMSO等剂型溶剂可以提高反应的产率而不会使催化剂失活。我们发现NMP作溶剂时,反应的产率最高,所以之后的研究中都使用NMP作为溶剂。
3楼2012-05-07 22:11:54
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