1-蒽酚的合成研究

Study on synthesis of 1-anthracenol

以蒽醌为起始原料,经混酸硝化,DMF精制,得到1-硝基蒽醌;用硫化钠还原,经DMF-水重结晶后得到1-氨基蒽醌;再在碱性溶液中经锌粉还原得到1-氨基蒽;最后用亚硫酸氢钠还原,经酸中和后用乙醇精制,得到1-蒽酚。所得的1-蒽酚结构经1H-NMR,IR等确证,总收率为22.6%,HPLC测定1-蒽酚的质量分数为97.7%。本合成方法成本低廉、工艺简单适合于工业生产。

Using anthraquinone as starting material, 1-nitroanthraquinone was synthesized by mixed acid nitration ,refining with dimethylforma mide. Reduction with sodium sulfide and then recrystallization from DMF-water gave 1-amiananthraquinone. 1-aminoanthraquinone was reduced with zinc powder in alkaline solution to give l-aminoanthracene. NaHSO3 was used to reduce 1-aminoan- thracene and neutralization was done with HCl,then 1-anthracenol was obtained by refining with ethanol. The structure of 1-anthracenol was confirmed by 1H-NMR, IR, etc, and total yield was 22. 6% with HPLC purity of 95.7%. The synthesis technology of l-anthracenol has the characteristics of inexpensive, simple and suitable for industrial production.