Department of Chemistry, Gebze Institute of Technology, PB.141, Gebze, 41400, Kocaeli, Turkey.
Dalton Trans. 2010 Nov 28;39(44):10685-91. doi: 10.1039/c0dt00818d. Epub 2010 Oct 11.
In this study, hexachlorocyclotriphosphazene, N(3)P(3)Cl(6) (cylotriphosphazene), was reacted with hydrophilic and hydrophobic groups to synthesize amphiphilic phosphazene derivatives (4-12). Cylotriphosphazene was reacted triethylene glycol monomethyl ether (TEGME), dipropylene glycol monomethyl ether (DPGME), diethylene glycol monobutyl ether (DEGBE), (1 : 3 mole proportion) in the presence of sodium hydride and using tetrahydrofuran (THF) as solvent at -60 °C. Three isomers (nongeminal cis-2,4,6 (1a-3a); nongeminal trans-2,4,6 (1b-3b); geminal 2,2,4 (1c-3c)) were isolated from the reaction of hexachlorocyclotriphosphazatriene (trimer) (1) with TEGME, DPGME and DEGBE. The substitution reactions of cis-tris isomers (1a-3a) with 4-amino butyric acid, 5-amino valeric acid and 6-amino hexanoic acid were separately done to provide amphiphilic phosphazenes (4-12). All compounds were characterized by using elemental analysis, (31)P NMR and mass spectroscopy. Thermosensitive properties of compounds were studied. The compounds (4-12) were soluble in both water and organic media that shows they are amphiphilic molecules. Concentration-dependent LCST (Lower Critical Solution Temperature) behaviours of new compounds (4-12) were measured in water. Compounds 7, 9, 11 and 12 exhibited a reversible and thermosensitive phase transition in aqueous medium, from soluble to insoluble states.
在这项研究中,六氯环三磷腈(N(3)P(3)Cl(6),三聚磷腈)与亲水和疏水基团反应,合成了两亲性磷腈衍生物(4-12)。在氢化钠存在下,使用四氢呋喃(THF)作为溶剂,在-60°C 下,将三聚磷腈与三乙二醇单甲醚(TEGME)、二丙二醇单甲醚(DPGME)、二乙二醇单丁醚(DEGBE)(摩尔比为 1:3)反应。从六氯环三磷三烯(三聚体)(1)与 TEGME、DPGME 和 DEGBE 的反应中分离出三种异构体(非顺式 2,4,6(1a-3a);非顺式 2,4,6(1b-3b);顺式 2,2,4(1c-3c))。对顺式三异构体(1a-3a)与 4-氨基丁酸、5-氨基戊酸和 6-氨基己酸的取代反应分别进行,得到两亲性磷腈(4-12)。所有化合物均通过元素分析、(31)P NMR 和质谱进行了表征。研究了化合物的热敏性质。化合物(4-12)在水和有机溶剂中均具有良好的溶解性,表明它们是两亲性分子。在水中测量了新化合物(4-12)的浓度依赖性 LCST(低临界溶液温度)行为。化合物 7、9、11 和 12 在水介质中表现出可逆和热敏相转变,从可溶状态变为不溶状态。