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以芦荟大黄素为原料,首先利用硫酸二甲酯对芦荟大黄素分子中的酚羟基进行选择性甲基化反应,合成1,8-二甲基氧芦荟大黄素,然后用氯铬酸吡啶盐(PCC)氧化甲基化的芦荟大黄素合成出1,8-二甲基氧芦荟大黄醛,最后使用丙酮和1,8-二甲基氧芦荟大黄醛进行Aldol缩合反应,合成了标题化合物,并用元素分析、质谱和1HNMR对所合成化合物的结构进行了表征。结果表明,使用丙酮作为溶剂,K2CO3为催化剂,在60~70℃下搅拌反应6~12 h,可以选择性、高产率得到1,8-二甲基氧芦荟大黄素。对于丙酮和1,8-二甲基氧芦荟大黄醛的Aldol缩合,超声波具有较好的促进效果。
To aloe emodin as raw material, the first use of dimethyl sulfate on the aloe-emodin molecular phenolic hydroxyl selective methylation reaction, synthesis of 1,8-dimethyl oxygen aloe-emodin, and then use pyridinium chlorochromate (PCC) to oxidize methylated aloe-emodin to synthesize 1,8-Dimethoxy aloe-aldehyde and finally Aldol condensation reaction using acetone and aloe-aldehyde of 1,8-dimethyl aldehyde to synthesize the title compound The structures of the synthesized compounds were characterized by elemental analysis, mass spectrometry and 1HNMR. The results showed that 1,8-Dimethoxy aloe-emodin could be obtained selectively and in high yield by using acetone as solvent and K2CO3 as catalyst under stirring at 60-70 ℃ for 6-12 h. For the Aldol condensation of acetone and 1,8-dimethyl oxalicol, the ultrasound has better promoting effect.