Using malononitrile as the raw material, a novel synthesis route of 2-amino-4,6-dimethoxypyrimidine(ADM) was put forward, in order to solve the instability in first step reaction of industrial synthesis. The influence...Using malononitrile as the raw material, a novel synthesis route of 2-amino-4,6-dimethoxypyrimidine(ADM) was put forward, in order to solve the instability in first step reaction of industrial synthesis. The influence of reactant ratio, temperature and time on product quality and yield was explored. The results showed that ADM was successfully prepared through acetyl chloride route, the yield was higher than that of industrial production process, and the process stability was good, with the product purity over 99%. Therefore, the new synthesis route is suitable for industrial production.展开更多
In order to get 2-chloro-4,6-dinitroresocinol(CDNR) with high purity,which influences the synthesis of 4,6-diaminoresorcinol dihydrochloride,the solubility of CDNR in various solvents was measured by laser method and ...In order to get 2-chloro-4,6-dinitroresocinol(CDNR) with high purity,which influences the synthesis of 4,6-diaminoresorcinol dihydrochloride,the solubility of CDNR in various solvents was measured by laser method and ethanol was chosen as the solvent.The recrystallization process of CDNR was investigated and crystallizing parameters such as cooling rate,temperature and time were discussed.Experimental results show that the time and temperature of crystallization greatly affect the yield and a higher yield can be received at-8 ℃ for 5 h.Slow cooling rate is helpful to the crystallization of CDNR,and the mechanical stirring or ultrasonic treatment can increase the yield and the purity of CDNR.展开更多
2-chloro-4,6-dinitroresorcinol was synthesized from 4,6-dinitro-1,2,3-trichlorobenzene by hydrolysis.The ultraviolet spectrophotometry was used to measure the absorbency of the hydrolysis mixture under different tempe...2-chloro-4,6-dinitroresorcinol was synthesized from 4,6-dinitro-1,2,3-trichlorobenzene by hydrolysis.The ultraviolet spectrophotometry was used to measure the absorbency of the hydrolysis mixture under different temperatures and periods of time.By kinetic calculation,it is shown that when the reaction temperature is in the range of 343.15 K to 358.15 K,the reaction is consistent with the secondary apparent dynamic model,the apparent activation energy is 200.11 kJ/mol and the expression of kinetic parameter k is 3.761×1028exp(-2.001×105/RT).The reaction is controlled by the course of chemical reactions.展开更多
文摘Using malononitrile as the raw material, a novel synthesis route of 2-amino-4,6-dimethoxypyrimidine(ADM) was put forward, in order to solve the instability in first step reaction of industrial synthesis. The influence of reactant ratio, temperature and time on product quality and yield was explored. The results showed that ADM was successfully prepared through acetyl chloride route, the yield was higher than that of industrial production process, and the process stability was good, with the product purity over 99%. Therefore, the new synthesis route is suitable for industrial production.
基金Sponsored by the Hi-Tech Research and Development Program of China(Grant No.2002AA305109)
文摘In order to get 2-chloro-4,6-dinitroresocinol(CDNR) with high purity,which influences the synthesis of 4,6-diaminoresorcinol dihydrochloride,the solubility of CDNR in various solvents was measured by laser method and ethanol was chosen as the solvent.The recrystallization process of CDNR was investigated and crystallizing parameters such as cooling rate,temperature and time were discussed.Experimental results show that the time and temperature of crystallization greatly affect the yield and a higher yield can be received at-8 ℃ for 5 h.Slow cooling rate is helpful to the crystallization of CDNR,and the mechanical stirring or ultrasonic treatment can increase the yield and the purity of CDNR.
基金the National Natural Science Foundations of China(Grant No.50333030)the Outstanding Youth Foundation of Heilongjiang Province of China(Grant No.JC04-12)
文摘2-chloro-4,6-dinitroresorcinol was synthesized from 4,6-dinitro-1,2,3-trichlorobenzene by hydrolysis.The ultraviolet spectrophotometry was used to measure the absorbency of the hydrolysis mixture under different temperatures and periods of time.By kinetic calculation,it is shown that when the reaction temperature is in the range of 343.15 K to 358.15 K,the reaction is consistent with the secondary apparent dynamic model,the apparent activation energy is 200.11 kJ/mol and the expression of kinetic parameter k is 3.761×1028exp(-2.001×105/RT).The reaction is controlled by the course of chemical reactions.
