合成化学
閤成化學
합성화학
CHINESE JOURNAL OF SYNTHETIC CHEMISTRY
2004年
4期
319-322
,共4页
程传杰%宋华付%陈玉岩%王玉生%丁绍民
程傳傑%宋華付%陳玉巖%王玉生%丁紹民
정전걸%송화부%진옥암%왕옥생%정소민
辅酶Q0%微波辐射%双氧水%3,4,5-三甲氧基苯甲醛%钼酸铵
輔酶Q0%微波輻射%雙氧水%3,4,5-三甲氧基苯甲醛%鉬痠銨
보매Q0%미파복사%쌍양수%3,4,5-삼갑양기분갑철%목산안
coenzyme Q0%microwave irradiation%hydrogen peroxide%3,4,5-trimethoxy benzaldehyde%ammonium molybdate
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43.8%.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50%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58.2%.辅酶Q0的结构经IR,1H NMR和13NMR确证.
以商用3,4,5-三甲氧基苯甲醛(Ⅰ)為起始原料, 通過兩步反應,閤成瞭輔酶Q0, 總收率達43.8%.第一步反應中,採用微波輻射改進瞭黃鳴龍還原法,以75.3%的收率製得3,4,5-三甲氧基甲苯(Ⅱ).第二步採用50%的雙氧水為氧化劑,鉬痠銨為催化劑,將Ⅱ直接氧化為輔酶Q0,收率為58.2%.輔酶Q0的結構經IR,1H NMR和13NMR確證.
이상용3,4,5-삼갑양기분갑철(Ⅰ)위기시원료, 통과량보반응,합성료보매Q0, 총수솔체43.8%.제일보반응중,채용미파복사개진료황명룡환원법,이75.3%적수솔제득3,4,5-삼갑양기갑분(Ⅱ).제이보채용50%적쌍양수위양화제,목산안위최화제,장Ⅱ직접양화위보매Q0,수솔위58.2%.보매Q0적결구경IR,1H NMR화13NMR학증.
Coenzyme Q0 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 Q0 in formic acid medium, catalyzed by ammonium molybdate, giving 58.2% yield. Coenzyme Q0 structure was confirmed by IR, 1H NMR and 13C NMR.