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采用异香兰醛和环己酮为原料,以乙醇为溶剂,在哌啶催化作用下羟醛缩合合成了姜黄素类抗癌药物重要中间体2-(E)-(3-羟基-4-甲氧基苯亚甲基)环己酮,通过1H NMR对产品的结构进行确证。并对反应条件进行了优化,优化条件为n(异香兰醛)∶n(环己酮)=1∶3,催化剂为哌啶,且质量为环己酮质量的20%,常压下70℃混合反应,反应结束后通过干法柱层析纯化,2-(E)-(3-羟基-4-甲氧基苯亚甲基)环己酮的反应收率达60.5%。通过扩展实验可知同样适用于香兰醛、3,4,5-三甲氧基苯甲醛等芳醛。
A new intermediate of 2- (E) - (3-hydroxy-4-methyl-4-methyloxanil), an important curcuminoid anticancer drug, was synthesized by the aldol condensation of isominal and cyclohexanone with ethanol as the solvent under the catalysis of piperidine. Oxybenzylidene) cyclohexanone, the structure of the product was confirmed by 1H NMR. The optimal reaction conditions were n (isanalanal): n (cyclohexanone) = 1: 3, the catalyst was piperidine and the mass was 20% of the mass of cyclohexanone, under the normal pressure of 70 ℃ After the reaction was completed, the reaction mixture was purified by dry column chromatography. The yield of 2- (E) - (3-hydroxy-4-methoxybenzylidene) cyclohexanone was 60.5%. By expanding the experiment we can see the same applies to vanillin, 3,4,5-trimethoxybenzaldehyde and other aromatic aldehydes.