电合成N,N-1,3-二甲基-4-氨基-5-甲酰氨基脲嗪的研究

Study on Electrosynthesis of N,N-1,3-Dimetyl-4-Amino-5-Formyl-Aminoureazine

研究了在甲酸溶液中,电还原N,N-1,3-二甲基-4-氨基紫脲酸(NAU)直接生成N,N-1,3-二甲基-4-氨基-5-甲酰氨基脲嗪(FAU), 将还原和酰化过程连续进行,减少了生产步骤,提高了生产效率。用正交实验法得到电还原NAU生成FAU的最佳条件:阴极液中含15%的甲酸、0.25mol·L-1NAU、2%硫酸铵;阳极液中含15%的甲酸;电流密度50mA·cm-2;温度30℃。化学反应温度104℃。在选定的最佳条件下,收率可达90%。

Synthesis of N,N-1,3-dimetyl-4-amino-5-formyl-aminoureazine by direct electro-reduction of N,N-1,3-dimetyl-4-amino-5-formyl-aminoureazine acid in the formic acid solution was studied. This method makes the processes of reduction and acylation carry through continously, which reduces the production procedure, and improves the production efficiency. The following optimize conditions of NAU抏lectro-reduction were gained through orthogonal experiments. In the cathode solution, formic acid抍oncentration is 15%, NAU抍oncentration is 0.25molL-1, concentration of ammonium sulfate is 2%; and in the anode solution, concentration of formic acid is 15%. The electrolysis temperature is 30C, current density is 50mAcm-2 and the acylation temperature is 140C. Under these optimize conditions, the yield of product may reach 90%.