一锅法绿色合成苯偶酰

doi:10.11944/j.issn.1000-0518.2016.11.160008

摘要/Abstract

摘要：

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¹H NMR、¹³C 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。

关键词: Salen催化剂, 苯偶姻, 苯偶姻, 苯偶酰, 催化氧化

Abstract:

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.

Key words: salen catalyst, benzoin, benzil, catalytic oxidation

谢康元, 陈强, 王佳耀, 林青青, 郑辉. 一锅法绿色合成苯偶酰[J]. 应用化学, 2016, 33(11): 1284-1288.

XIE Kangyuan, CHEN Qiang, WANG Jiayao, LIN Qingqing, ZHENG Hui. One-pot Green Synthesis of Benzil[J]. Chinese Journal of Applied Chemistry, 2016, 33(11): 1284-1288.

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