Magnetic nanoparticle-supported phosphoramidite catalyst and preparation method thereof and preparation method of γ,δ-unsaturated ketone
A magnetic nanoparticle and phosphoramidite technology, applied in the field of catalysts and organic synthesis, can solve the problems of low catalyst activity, low product selectivity, and high reaction temperature, and achieve high catalyst activity, simple preparation process, and simple operation of reaction conditions. Effect
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Embodiment 1
[0055] Example 1: SiO 2 @Fe 3 O 4 preparation
[0056] Under the argon atmosphere, take the nano-iron tetroxide dispersion (10~50nm, 20wt% in H 2 O) 100 mL, add 300 mL of ethanol, 2 mL of ammonia (25%) and 2 mL of oleic acid. Sonicate for 0.5-1.0 h, add dropwise 40 g of ethyl orthosilicate in ethanol (0.5 g / mL), stir at room temperature for 12 h, and apply a magnetic field to separate SiO 2 @Fe 3 O 4 , washed three times with ethanol, and stored under argon atmosphere.
Embodiment 2
[0057] Example 2: Preparation of Silane Coupling Agent Coupling-1 Containing Phosphoramidate Group
[0058]
[0059] Under an argon atmosphere, add anhydrous toluene (105.49g), pyridine (8.71g, 0.11mol) and phenyl dichlorophosphate (10.55g, 0.05mol) to a 250ml Schlenk bottle, turn on stirring, put the Schlenk bottle into -10 ℃, the temperature of the mixed solution in the bottle was lowered to -10℃. The silane coupling agent UPTMS (13.34 g, 0.06 mol) was slowly added dropwise with a constant pressure dropping funnel (dropping time was about 30 min), and the temperature of the reaction solution in the Schlenk bottle was controlled between -10 and 0 °C during the dropping process. After the dropwise addition, the reaction was carried out at 30° C. for 1 h, deionized water (1.08 g, 0.06 mol) was added, and the reaction was carried out at room temperature for 0.5 h to terminate the reaction. The reaction solution was filtered, the filtrate was distilled under reduced pressure ...
Embodiment 3
[0061] Example 3: Preparation of Silane Coupling Agent Coupling-2 Containing Phosphoramidate Groups
[0062]
[0063] Under an argon atmosphere, add anhydrous toluene (105.49g), pyridine (9.89g, 0.13mol) and phenyl dichlorophosphate (10.55g, 0.05mol) to a 250ml Schlenk bottle, turn on stirring, put the Schlenk bottle into -10 ℃, the temperature of the mixed solution in the bottle was lowered to -10℃. The silane coupling agent APTMS (11.65 g, 0.065 mol) was slowly added dropwise with a constant pressure dropping funnel (dropping time was about 30 min), and the temperature of the reaction solution in the Schlenk bottle was controlled between -10 and 0 °C during the dropping process. After the dropwise addition, the reaction was carried out at 30° C. for 1 h, deionized water (1.35 g, 0.075 mol) was added, and the reaction was carried out at room temperature for 0.5 h to terminate the reaction. The reaction solution was filtered, the filtrate was distilled under reduced pressu...
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