belstaff bolsas Synthetic broad-spectrum antimicro

lin06900 · Wysłany: Wto 19:37, 22 Mar 2011

Ultrasonic synthesis of broad-spectrum antimicrobial agent Domiphen

Planning project (2008); Xuzhou Medical College Hospital topics (08KJ35) of Xuzhou Medical College ACTAACADEMIAEMEDICINAEXUZHOU2009, 29 ( Cool

O / 7/cH32 Results and analysis 2.1 sonication of reaction temperature and the choice of solvent sonication of different temperature on the reaction rate in Table 1. The results showed that the reaction temperature conducive to the reaction temperature reached 100 ~ C, the reaction speed, continue to rise little effect of temperature on reaction rate and the temperature is too high, the product of good color and crystal form, therefore, Select this study the reaction at 100 ℃. Table 1 Ultrasound of reaction temperature on reaction rate to meet the requirements of industrial production,[link widoczny dla zalogowanych], should be inexpensive and easy to select the solvent for the reaction solvent recovery. Taking into account the ethyl acetate, low boiling point solvents such as acetone,[link widoczny dla zalogowanych], is not conducive to recovery, and easily controlled system of acetone as the solvent of drugs, so the present study, toluene as solvent, reaction temperature and help to improve the dispersion of reactants, reaction to avoid local temperature is too high and the product turn yellow. 2.2 mole ratio of the choice of different mole ratio on the yield and quality of the data in Table 2. Conventional synthetic methods, B a bromobenzene ether: N, N-methyl-second or two when the tertiary amine = 1:1.1 high yield,[link widoczny dla zalogowanych], good crystal. Ultrasonic synthesis methods, molar ratio l: 1 and 1:1.1 final yield could be higher, but the molar ratio of 1:1.1, the darker color of the crude product obtained, after the step of re-crystallization higher requirements. In addition, from a cost point of view, the best material for ultrasonic reaction molar ratio of 1:1. Table 2 molar ratio of 2.3 on the product quality of different reaction, the crude product yield and appearance of Table 3 shows, ultrasound and conventional synthesis methods of synthetic crude product yield no significant difference, but the conventional synthesis method to get the crude product appearance and melting point of crystal poor, which may be due to the product in the package are not complete response to N, N-methyl-second or two tertiary amines. In the ultrasound,[link widoczny dla zalogowanych], because it produces secondary effects such as mechanical vibration, diffusion, solid break and so broken in favor, so the product of the crystallization process in the small parcels of impurities by simple washing can remove most of the impurities, Therefore, the crude product obtained by sonication lighter color, high melting point. Meanwhile, the ultrasonic response time than conventional synthetic methods shorten, the reason may be due to mechanical vibration under ultrasound, is conducive to the spread of reactants, mixing process, thus speeding up the reaction speed. Table 3 on the reaction of different reaction time and the quality of the crude product recrystallized 2.4 on product quality and yield of the reaction process to remove impurities and improve the crystal Domiphen products,[link widoczny dla zalogowanych], color and melting point, the experiment re- crystal operation (Table 4). Conventional synthetic methods to achieve the quality requirements in need of re-crystallized three times, while the ultrasonic synthesis of the products were only once in the recrystallization solvent, the product showed a melting point in good condition and appearance, the total yield higher than that of conventional synthetic methods. Table 4 re-crystallization of the product quality and yield of 3 Conclusion The experiment found that ultrasound method is better than conventional synthetic Domiphen synthesis. In the ultrasonic synthesis process, with toluene as solvent, temperature 100 ~ C, the reaction of 1h to get optimum color, the degree of citrate, the crude product can only be the appearance of a re-crystallization, melting more excellent products, and the yield up to 90%.
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