微波辐射法合成辅酶Q_0(英文)

Synthesis of Coenzyme Q_0 under Microwave Irradiation

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

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.