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本研究报道了一条经济、绿色的工艺路线合成双醋瑞因(1)。1,8-二羟基-3-羟甲基-9,10-蒽醌(2)经2-碘酰基苯甲酸氧化,高收率(90%)得到4,5-二羟基-9,10-蒽醌-2-甲醛(3);再以DMSO为溶剂,经Pinnick氧化反应得4,5-二羟基-9,10-蒽醌-2-羧酸(4),收率85%;4在酸性条件下乙酰化得1,总收率54.2%(以2计),纯度99.77%。本工艺不仅避免了重金属残留的问题,革除了易燃易爆氧化试剂的使用,且反应条件温和、操作简便,更适合工业生产的需求。本路线中由2制备4的方法未见文献报道。
This study reports on an economical, green process route for the synthesis of diacerein (1). 1,8-Dihydroxy-3-hydroxymethyl-9,10-anthraquinone (2) was oxidized with 2-iodoxybenzoic acid to give 4,5-dihydroxy-9,10- Anthraquinone-2-carboxaldehyde (3); 4) dihydroxy-9,10-anthraquinone-2-carboxylic acid (4) was obtained by Pinnick oxidation with DMSO as solvent, yield 85% Acetylation under acidic conditions 1, the total yield of 54.2% (2), the purity of 99.77%. The process not only avoids the problem of heavy metal residue, but also eliminates the use of flammable and explosive oxidation reagents, and the reaction conditions are mild, easy to operate and more suitable for industrial production. The method of preparation 4 from this route has not been reported in the literature.