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以2,3-二氢-1,4,5,8-四羟基蒽醌和N,N-二甲基乙二胺为原料,合成了抗癌药物1,4-二[2-(二甲胺基)乙胺基]-5,8-二羟基蒽醌(下称:AQ4),考察了温度、溶剂、催化剂、氧化方式等对其产品收率的影响.确定的较佳工艺方法为:以2,3-二氢-1,4,5,8-四羟基蒽醌和N,N-二甲基乙二胺为起始原料进行缩合反应,用N,N-二甲基乙二胺兼做溶剂,首先制得1,4-二[2-(二甲胺基)乙胺基]-5,8-二羟基蒽醌隐色体(AQ4隐色体),进而用硝基苯进行氧化反应制得AQ4,产品总收率达到67.5%,产品结构利用红外(IR)、核磁(1H NMR)进行了表征.较佳的缩合反应条件为:反应温度50~55℃、反应时间2 h;较佳的氧化反应条件为:反应温度140~145℃、回流反应时间15 min.
Using 2,3-dihydro-1,4,5,8-tetrahydroxyanthraquinone and N, N-dimethylethylenediamine as raw materials, the anti-cancer drug 1,4-bis [2- Amino) ethylamino] -5,8-dihydroxyanthraquinone (AQ4), the effects of temperature, solvent, catalyst and oxidation mode on the yield of the product were investigated. The optimum process was determined as follows: With 2,3-dihydro-1,4,5,8-tetrahydroxyanthraquinone and N, N-dimethylethylenediamine as the starting material for condensation reaction, with N, N-dimethylethylenediamine Also as a solvent, first, 1,4-bis [2- (dimethylamino) ethylamino] -5,8-dihydroxyanthraquinone leuco (AQ4 leuco) was prepared and further treated with nitrobenzene AQ4 was obtained by oxidation reaction, the total yield of the product reached 67.5%, and the product structure was characterized by IR and 1H NMR.The optimum reaction conditions were: reaction temperature 50 ~ 55 ℃, reaction time 2 h ; The preferred oxidation conditions are: reaction temperature 140 ~ 145 ℃, reflux reaction time 15 min.