Polycatenar ligands and hybrid nanoparticles made therefrom
A nanoparticle, compound technology, applied in the fields of nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, which can solve the problems of rare earth nanoparticle morphology and monodispersity dependence
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[0225] Reagents and materials used in the following examples were obtained from commercial sources or synthesized from commercially available reagents and compounds unless otherwise stated. Reagents and materials used in the following examples are summarized below.
[0226] 1-octadecene (90%), oleylamine (80%-90%), chloroauric acid (HAuCl 4 ·3H 2 O; ACS reagent), oleylamine (80%-90%), 1,2,3,4-tetralin (tetralin, 98+%), copper(II) sulfate pentahydrate (98+%) and 2,6-Di-tert-butyl-4-picoline (98%) was purchased from Acros. Oleic acid (90%), cadmium acetylacetonate (99.9%), 1,2-dodecanediol (90%), tributylphosphine (97%), trioctylphosphine (90%), selenium powder ( 99.99%), sulfur powder (99.99%), diphenylphosphine (97%), selenium particles (99.999%), zinc acetate dehydrate (99.999%), iron (III) acetylacetonate (99.9%), oleyl alcohol ( 60%), octyl ether (99%), tris(trimethylsilyl)phosphine (95%), lead oxide (99.9%), indium acetylacetonate (99.99%), tert-butylamine borane compl...
example 1
[0243] Example 1. Synthesis of end groups
[0244] The steps used to synthesize the end groups 5a-5e used in the compounds of the present invention are summarized in Scheme 3, where A, B, C and D refer to the general procedures described therein.
[0245] Option 3.
[0246]
[0247] Methyl 3,4,5-tris(octadecyloxy)benzoate (compound 2a) was prepared according to the general procedure designated as General Procedure A below. To a stirred solution of methyl 3,4,5-trihydroxybenzoate 1a (5 g, 27.0 mmol) and 1-bromooctadecane (32.6 g, 97.8 mmol) in DMF (100 mL) was added K 2 CO 3 (14.9g, 108.0mmol) and KI (0.45g, 2.7mmol), and the resulting mixture was stirred at 90°C for 12h. The reaction mixture was cooled and washed with CHCl 3 (200mL) diluted with H 2 O (3×50mL) washed over anhydrous MgSO 4 Dry, filter, and concentrate the filtrate under reduced pressure. Redissolve the residue in as little warm CHCl as possible 3 , and mixed with MeOH to induce precipitation. The pr...
example 2
[0277] Example 2. Formation of Compounds of the Invention
[0278] Azide or alkyne functionalized end groups prepared according to Example 1 were linked together with azide or alkyne functionalized surface anchoring groups using Huisgen cycloaddition reaction in the presence of copper catalyst and sodium ascorbate, These surface anchoring groups are generally obtained from commercial sources unless otherwise stated.
[0279] The general procedure designated as General Procedure E for carrying out cycloaddition reactions is as follows. To azide (2.77mmol), alkyne (3.3mmol) and CuSO 4 ·5H 2 O (0.21g, 0.83mmol) in THF / H 2Sodium ascorbate (0.22 g, 1.11 mmol) was added to a stirred solution in O=4:1 (6 mL), and the resulting mixture was stirred at 75° C. under microwave irradiation (isothermal mode) for 3 h. The solvent was evaporated and the residue was dissolved in CHCl 3 (100 mL) and washed with 1N HCl (3 x 100 mL). in anhydrous Na 2 SO 4 The organic layer was dried on ,...
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