Faculty of Natural Science, Institute of Chemistry, Department of Inorganic Chemistry, Chemnitz University of Technology, Chemnitz, Germany.
J Colloid Interface Sci. 2011 Jul 15;359(2):454-60. doi: 10.1016/j.jcis.2011.03.092. Epub 2011 Apr 2.
The preparation and characterisation of a series of well-defined low generation (poly)amidoamine (PAMAM)-based dendrimers with end-grafted ethylene glycol ether moieties of type N(CH(2)CH(2)C(O)NHCH(2)CH(2)NR(2))(3) (3a, R=CH(2)CH(2)C(O)OCH(2)CH(2)OCH(3); 3b, R=CH(2)CH(2)C(O)O(CH(2)CH(2)O)(2)C(2)H(5); 3c, R=CH(2)CH(2)C(O)O(CH(2)CH(2)O)(9)CH(3)), CH(2)N(CH(2)CH(2)C(O)NHCH(2)CH(2)NR(2))(2) (4, R=CH(2)CH(2)C(O)O(CH(2)CH(2)O)(2)C(2)H(5)) and (R(2)NCH(2)CH(2)NHC(O)CH(2)CH(2))NCH(2)CH(2)N(CH(2)CH(2)C(O)NHCH(2)CH(2)NR(2))(2) (5a, R=CH(2)CH(2)C(O)OCH(2)CH(2)OCH(3); 5b, R=CH(2)CH(2)C(O)O(CH(2)CH(2)O)(2)C(2)H(5); 5c, R=CH(2)CH(2)C(O)O(CH(2)CH(2)O)(9)CH(3)) and their application for the stabilisation of gold nanoparticles (Au NPs) is described. These dendrimers were prepared by a consecutive divergent synthesis methodology including Michael addition and amidation cycles. For comparison, amidoamine related model compounds N(C(3)H(7))R(2) (1, R=CH(2)CH(2)C(O)O(CH(2)CH(2)O)(2)C(2)H(5)) and CH(2)NR(2) (2, R=CH(2)CH(2)C(O)O(CH(2)CH(2)O)(2)C(2)H(5)) were also synthesised to estimate the minimum required donating capabilities of the stabiliser. Loading the appropriate dendritic templates with H[AuCl(4)] (12) and subsequent reduction of the respective metallodendrimers with Na[BH(4)] produced dendrimer encapsulated gold colloids. The dendrimeric scaffold, the length of the ethylene glycols, the adjusted stabilizer:gold ratio and the duration of reaction time affects the average Au particle diameter in a range of 4.0 (±0.9) to 58.5 (±14.5) nm. Furthermore, depending on the nature of the stabiliser, nanoparticles were formed having spherical or multiple morphologies. Characterisation by transmission electron microscopy (TEM), dynamic light scattering (DLS), UV/vis, and IR spectroscopy revealed that Au NPs are formed and protected inside the dendrimer scaffold.
描述了一系列具有明确低代（聚）酰胺胺（PAMAM）结构的树枝状分子的制备和特性，这些分子的末端接枝有乙撑基亚乙基醚基团，类型为 N(CH(2)CH(2)C(O)NHCH(2)CH(2)NR(2))(3)（3a，R=CH(2)CH(2)C(O)OCH(2)CH(2)OCH(3)；3b，R=CH(2)CH(2)C(O)O(CH(2)CH(2)O)(2)C(2)H(5)；3c，R=CH(2)CH(2)C(O)O(CH(2)CH(2)O)(9)CH(3)），CH(2)N(CH(2)CH(2)C(O)NHCH(2)CH(2)NR(2))(2)（4，R=CH(2)CH(2)C(O)O(CH(2)CH(2)O)(2)C(2)H(5))和（R(2)NCH(2)CH(2)NHC(O)CH(2)CH(2))NCH(2)CH(2)N(CH(2)CH(2)C(O)NHCH(2)CH(2)NR(2))(2)（5a，R=CH(2)CH(2)C(O)OCH(2)CH(2)OCH(3)；5b，R=CH(2)CH(2)C(O)O(CH(2)CH(2)O)(2)C(2)H(5)；5c，R=CH(2)CH(2)C(O)O(CH(2)CH(2)O)(9)CH(3)），并描述了它们在稳定金纳米粒子（Au NPs）方面的应用。这些树枝状分子是通过连续的发散合成方法制备的，包括迈克尔加成和酰胺化循环。为了进行比较，还合成了与酰胺胺相关的模型化合物 N(C(3)H(7))R(2)（1，R=CH(2)CH(2)C(O)O(CH(2)CH(2)O)(2)C(2)H(5)）和CH(2)NR(2)（2，R=CH(2)CH(2)C(O)O(CH(2)CH(2)O)(2)C(2)H(5)），以估计稳定剂所需的最小供电子能力。用 H[AuCl(4)]（12）加载适当的树枝状模板，并随后用 Na[BH(4)]还原相应的金属树枝状分子，得到了树枝状包裹的金胶体。树枝状支架、乙撑基亚乙基醚的长度、调整的稳定剂：金比和反应时间都会影响平均 Au 粒子直径在 4.0（±0.9）到 58.5（±14.5）nm 之间。此外，根据稳定剂的性质，形成了具有球形或多种形态的纳米颗粒。透射电子显微镜（TEM）、动态光散射（DLS）、紫外/可见和红外光谱的表征表明，Au NPs 是在树枝状支架内形成和保护的。
