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以水为反应介质,水合肼为还原剂,研究了痕量铜催化3-甲基蒽醌-[1,2-c]-异噁唑还原开环反应以清洁高效合成1-氨基-2-乙酰基蒽醌,考察了不同种类过渡金属硝酸盐的催化性能,发现Cu(NO3)2性能最好.加入2.6%的催化剂和1.3倍的水合肼,在室温反应2 h,底物转化率和目标产物选择性分别可达到97.2%和95%,TON达到38.产品结构经氢核磁谱和质谱得以确证,主要副产为羟基取代的1-氨基-2-乙酰基蒽醌.此外,提出了铜催化3-甲基蒽醌-[1,2-c]-异噁唑还原开环反应合成1-氨基-2-乙酰基蒽醌的可能反应机理.
With water as the reaction medium and hydrazine hydrate as reductant, a trace copper-catalyzed reduction reaction of 3-methylanthraquinone- [1,2-c] -isoxazole was studied to purify 1-amino-2- Acetylanthraquinone, the catalytic properties of different kinds of transition metal nitrates were investigated and it was found that Cu (NO3) 2 had the best performance. After adding 2.6% of catalyst and 1.3 times of hydrazine hydrate at room temperature for 2 h, The selectivity of the target product was 97.2% and 95%, respectively, TON reached 38. The structure of the product was confirmed by proton nuclear magnetic resonance and mass spectrometry, the main byproduct hydroxy-substituted 1-amino-2-acetylanthraquinone. In addition, Possible Catalytic Mechanism for the Synthesis of 1-Amino-2-Acetylanthraquinone by Copper-Catalyzed Reduction of 3-Methylanthraquinone- [1,2-c] -isoxazole to Ring-Opening Reaction.