Method for synthesizing three direction dendrimer core by microwave
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A technology of microwave synthesis and molecular nucleus, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of delaying the synthesis cycle of dendrimers, taking a long time, increasing synthesis costs, etc., and shortening the synthesis reaction time , large radiation energy, and the effect of increasing productivity
Inactive Publication Date: 2009-11-18
WUHAN INSTITUTE OF TECHNOLOGY
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However, these reactions are all time-consuming when conventional methods are used for synthesis at present, and there is also the problem of low yield in the step of nitrile alcoholysis,
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Embodiment 1
[0046] (1) Dissolve 1 g of triethanolamine in 10 ml of 1,4-dioxane, add potassium hydroxide aqueous solution (9 mmol KOH / 2.5 ml H 2 O), stir well, add 80mg 18-crown-6 ether;
[0047] (2) add 0.02mol acrylonitrile;
[0048] (3) The reaction vessel was placed in a microwave reactor, heated to reflux for 30 min under 325W microwave irradiation, the reaction was stopped, and 1.480 g of trinitrile was obtained by column chromatography, yield: 71.62%.
Embodiment 2
[0050] (1) Dissolve 1 g of triethanolamine in 10 ml of 1,4-dioxane, add potassium hydroxide aqueous solution (9 mmol KOH / 2.5 ml H 2 O), stir well, add 80mg 18-crown-6 ether;
[0051] (2) add 0.03mol acrylonitrile;
[0052] (3) The reaction vessel was placed in a microwave reactor, heated to reflux for 50 min under 195W microwave irradiation, the reaction was stopped, and 1.490 g of trinitrile was obtained by column chromatography, yield: 72.08%.
Embodiment 3
[0054] (1) Dissolve 1 g of triethanolamine in 10 ml of 1,4-dioxane, add potassium hydroxide aqueous solution (9 mmol KOH / 2.5 ml H 2 O), stir well, add 80mg 18-crown-6 ether;
[0055] (2) add 0.06mol acrylonitrile;
[0056] (3) The reaction vessel was placed in a microwave reactor, heated to reflux for 70 min under 65W microwave irradiation, the reaction was stopped, and 1.499 g of trinitrile was obtained by column chromatography, yield: 72.53%.
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Abstract
The invention relates to a method for synthesizing three direction dendrimer core by microwave, comprising the following steps: synthesizing dinitrile: dissolving trolamine in a reaction vessel with 1,4-dioxane, adding a strong base catalyst and a crown ether phase transfer catalyst; then adding acrylonitrile in the reaction system, placing the solution in a microwave reactor for microwave irradiation to obtain dinitrile; synthesizing triester: dissolving the obtained dinitrile in a reaction vessel with methanol, adding concentrated sulphuric acid; placing the solution in the microwave reactor for microwave irradiation to obtain triester; synthesizing triamine: dissolving the obtained triester in a reaction vessel with methanol, adding ethylene diamine; placing the solution in the microwave reactor for microwave irradiation to obtain three direction dendrimer core. Compared with the existing art, the invention has the following advantages: the radiation energy is large by microwave heating, the synthetic reaction time of dendrimer core is effectively shortened; the productivity can be obviously improved, which is obvious for the alcoholysis of nitrile.
Description
technical field [0001] The invention relates to a method for synthesizing a three-directional dendritic molecular nucleus by microwave. Background technique [0002] Dendrimers are a new class of synthetic macromolecules, and their many unique properties have attracted widespread attention in related fields in recent years. It has the characteristics of high geometric symmetry, precise molecular structure, low dispersion coefficient, a large number of surface functional groups, and controllable internal cavity and molecular size. It can be used in many fields such as catalysis, drug metabolism, and gene carrier. . [0003] The research results show that, among many dendrimers, polyamide-amine dendrimers are open and relatively loose structures at low generation (below 3 generations), and are closely packed on the surface at high generation (more than 4 generations). structure. The molecular size of polyamide-amine dendrimer is in the nanometer range, and the molecular siz...
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