Microwave Synthesis of Dendrimer Polyamide-amine Solution

Dendrimer molecule (PAMAM) is a kind of three-dimensional, highly ordered, widely used lame molecule and can be used in many fields such as catalysis, drug metabolism, surfactants and so on. Some researchers use surface fluorescent probes to study the properties of these polymers by surface modification. Studies have shown that 4.0G with 1VH2S end group polyamide-amine itself has strong fluorescence properties. Since the first time in 1985, Tomamia W proposed a stepwise polymerization method to synthesize PAMAM, there have been many methods such as divergence method, convergence method, and solid phase synthesis. However, most of them have the disadvantages of long reaction time, complicated operation, and low cost. In recent years, as a new synthesis method, microwave has attracted much attention from the chemical industry at home and abroad. It has been widely used in organic synthesis, synthesis of inorganic materials, molecular sieve synthesis, and assembly of some inorganic materials. In this paper, the synthesis of polyamine amine-amine oxime molecule by microwave method is reported. By studying the fluorescence properties of the product, 40 and 40 min are the most suitable reaction conditions. This new PAMAM synthesis method is fast, the product is homogeneous, and the fluorescence intensity is high.

1. Reagents required for the synthesis experiment: Ethylenediamine (EDA), AR, Tianjin Fuchen Chemical Reagent Factory; Methyl Acrylate (MA Tianjin Chemical Reagent Co., Ltd.; anhydrous methanol, AR, Tianjin Guangfu Fine Chemical Research Institute 2 Microwave digester; United States PerkinElmer-1555 fluorescence analyzer; FT-80A NMR 1.2 Synthesis of different generations of PAMAM by Michael addition reaction and hydrazine amination reaction alternately obtained.

At room temperature, certain children's methanol and ethylenediamine were mixed in a round bottom flask, and the methyl methacrylate was dropped under magnetic stirring. The mixed solution was placed in a microwave to heat up the temperature, removed, and cooled. Distillation under reduced pressure at 22 and 72, respectively, yields half-generation and whole-generation products.

Under the same conditions, the microwave program was heated up to 35, 40t, 45, 50, 55, respectively, and the 0.5G product was diluted to the same multiple. The fluorescence intensity was measured as shown in the following figure (1): 1.2.2 Different microwave heating time experiments The 5G product was diluted with the same multiples and the fluorescence intensity was measured as shown in the following figure (2): 2 Structure and Characterization The NMR displacement measurement was consistent with that of 5, indicating that the chemical structure of the synthesized product in the microwave was consistent with the traditional method. 1 H NMR spectrum results and discussion The traditional method for synthesizing dendritic amine molecule polyamidoamine takes a long time, and the reaction is mostly carried out at low temperature, it is not easy to operate, and the fluorescence properties of the related products are only a few. The research team mentioned it. The synthesis of PAMAM by microwave method at 40 °C for 40 min greatly shortens the reaction time. The fluorescence efficiency of the product can be more easily used to commercialize PAMAM synthesis, and its fluorescence properties are used to extend its labeling on biomolecules. , Chemical modification and other fields of application.