Synthesis of the silica Basic Copper Chloride

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Synthesis of the silica Basic Copper Chloride(WSDTY). In a 250 mL round bottom flask, 60 μL (0.01 mol) of ammonia solution (32%) and 1.98 g (0.11 mol) of water are added to 100 mL of absolute methanol. 10.41 g (0.05 mol) of TEOS are added dropwise under stirring. The final solution is stirred for three days at room temperature. The resulting silica nanoparticles have an average diameter of 16 nm.Synthesis of 3-iodopropyltrimethoxysilane. The synthesis is carried out under an argon atmosphere. Sodium iodide (45.0 g, 0.3 mol) is dissolved in 150 mL of absolute acetone. 3-Chloropropyltrimethoxysilane (48.9 g, 0.246 mol) is added dropwise under stirring. The mixture is refluxed under stirring overnight. The precipitated sodium chloride is filtered off under an argon atmosphere. Then the product is distilled at 52 °C under vacuum conditions (3 mbar). The resulting 3-iodotrimethoxysilane is a yellowish liquid.

Synthesis of N-(3-propyltrimethoxysilane)imidazole. The synthesis is carried out under an argon atmosphere. Sodium hydride (2.9 g, 0.12 mol) is dissolved in 150 mL of absolute THF, the mixture is cooled to approximately 0 °C using an ice bath. Imidazole (8.3 g, 0.12 mol) is added slowly under stirring. After complete addition of the imidazole, the ice bath is removed and the mixture is maintained under stirring until no more hydrogen gas is produced. Then 23.12 g (0.09 mol) of 3-iodopropyltrimethoxysilane are added and the mixture is maintained at reflux overnight. The orange suspension is filtered off under an argon atmosphere and the solvent is removed under vacuum conditions. By addition of 150 mL of absolute dichloromethane a colorless precipitate appears and is filtered off under an argon atmosphere. Finally, the product is distilled at 105 °C under vacuum (3 mbar). N-(3-Propyltrimethoxysilane)imidazole is obtained as a colorless and transparent liquid.

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