以绿色廉价的乙醇-水为溶剂,一锅法合成了金属萨伦(Salen)配体催化剂[M(Salen)](M=Co,Cu, Zn,Fe,Mn),完成了安息香氧化制备苯偶酰。产物结构通过1 H NMR、13 C NMR、IR、HRMS及XRD等技术手段进行了表征。通过正交设计实验考察了催化剂质量浓度、反应时间、溶剂、反应温度、KOH质量浓度等因素对反应的影响,获得了最优条件。实验结果表明,以[Co(Salen)]作为催化剂(1.7×10-3 g/mL),80%(体积分数)乙醇作为溶剂,70℃,反应50 min,苯偶酰产率达到76.5%。催化剂循环使用5次,苯偶酰收率仍可达74.2%。为绿色制备苯偶酰提供了一种新途径。
One-pot green synthesis of benzil catalyzed by Co ( Salen ) from benzoin in alcohol-water was developed.The products was confirmed by 1H NMR, 13C NMR, IR, HRMS and XRD.The orthogonal experimental design gives the optimal reaction conditions about the catalyst loading , reaction time, solvents, reaction temperature , and the amount of potassium hydroxide .The best conditions is Co ( Salen ) catalyst , 80% alcohol-water, 50 minutes and 70 ℃.The highest yield of 76.5% could be obtained under that conditions.The catalyst can be recycled at least five times up to the 74.2% yield.It is a green method and novel protocol to synthesize benzil .
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