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微波辐射法合成辅酶Q₀（英文）

Synthesis of Coenzyme Q₀ under Microwave Irradiation

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【Author】 CHENG Chuan-jie 1, SONG Hua-fu 1, CHEN Yu-yan 1, WANG Yu-sheng 1, DING Shao-min 2 (1. Research Center of Materials Science, Beijing Institute of Technology, Beijing 100081, China; 2. Beijing Chunfu Research Center of Applied Technology, Beijing 100095, China)

【机构】北京理工大学材料科学研究中心；北京春甫应用技术研究中心北京100081；北京100081；北京100095；

【摘要】以商用 3,4 ,5 三甲氧基苯甲醛 (Ⅰ )为起始原料 ,通过两步反应 ,合成了辅酶Q0 ,总收率达 4 3.8%。第一步反应中 ,采用微波辐射改进了黄鸣龙还原法 ,以 75 .3%的收率制得 3,4 ,5 三甲氧基甲苯 (Ⅱ )。第二步采用 5 0 %的双氧水为氧化剂 ,钼酸铵为催化剂 ,将Ⅱ直接氧化为辅酶Q0 ,收率为 5 8.2 %。辅酶Q0 的结构经IR ,1HNMR和13 NMR确证更多还原

【Abstract】 Coenzyme Q 0 was prepared via two steps using commercially available 3,4,5-trimethoxy benzaldehyde as the starting material. The overall yield has reached 43.8%. In the first step, Huang-Minlon reduction methodology was modified by the use of microwave irradiation, which afforded 3,4,5-trimethoxy toluene in 75.3% yield. In the second step, 50% hydrogen peroxide proved to be powerful in oxidizing 3,4,5-trimethoxy toluene to coenzyme Q 0 in formic acid medium, catalyzed by ammonium molybdate, giving 58.2% yield. Coenzyme Q 0 structure was confirmed by IR, 1H NMR and 13C NMR.更多还原