Preparation method and application of meso-porous silicon material-immobilized chiral gold catalyst
A technology of gold catalyst and mesoporous silicon, which is applied in the field of preparation of heterogeneous mesoporous silicon material immobilized chiral gold catalyst, can solve the problem that gold heterogeneous catalysts are easy to be oxidized, there are few researches on heterogeneous catalysis, and the limitation of catalyst application and other problems, to achieve the effects of easy separation, simple synthesis steps, huge development potential and application prospects
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Embodiment 1
[0019] (1) Preparation of styryl functionalized chiral phosphine ligands
[0020] Weigh 1g (5.0mmol) of sulfenamide phosphine ligand and 20mL of dichloromethane in a flask, place it in a low-temperature constant temperature reaction bath at -48°C, slowly drop 10mmol of styrene into the round-bottomed flask, and the addition is complete Afterwards, the device was transferred to room temperature and reacted for 9 h with NH 4 Cl solution was used to quench the reaction, then diluted with 3×10 mL ethyl acetate, extracted, dried with anhydrous sodium sulfate, spin-dried and separated by column chromatography to obtain 0.8 g product which was styryl-functionalized chiral phosphine ligand .
[0021] (2) Preparation of functionalized mesoporous silicon materials
[0022] Under an argon atmosphere, weigh 216 mg of the above-prepared chiral phosphorus ligand, 1.0 g of mercapto-functionalized SBA-15, and 54 mg of AIBN in a flask, add 100 mL of toluene after vacuuming, and reflux at 100...
Embodiment 2
[0028] (1) Preparation of allyl functionalized chiral phosphine ligands
[0029] Weigh 5.0mmol of sulfenamide phosphine ligand and 20mL of dichloromethane in a flask, place it in a low-temperature constant temperature reaction bath at -48°C, slowly drop 10mmol of allylmagnesium bromide into the flask, and after the dropwise addition , transfer the device to room temperature and react with NH for 8h 4 Cl solution was used to quench the reaction, then diluted with 3×10 mL ethyl acetate, extracted, dried with anhydrous sodium sulfate, spin-dried and separated by column chromatography to obtain 0.9 g product which was allyl functionalized chiral phosphine ligand .
[0030] (2) Preparation of functionalized mesoporous silicon materials
[0031] Under an argon atmosphere, weigh 230 mg of the above-prepared chiral phosphine ligand, 1.0 g of mercapto-functionalized SBA-15 and 56 mg of AIBN in a flask, add 100 mL of toluene after vacuuming, and reflux at 95°C for 7 hours. After suct...
Embodiment 3
[0035] (1), preparation of binaphthylvinyl functionalized chiral phosphine ligands
[0036] Take 5.0 mmol of sulfenamide phosphine ligand and 20 mL of dichloromethane in a flask, place it in a low-temperature constant temperature reaction bath at -48 ° C, slowly drop 10 mmol of binaphthylethylene magnesium bromide into the flask, and after the addition is complete, Transfer the device to room temperature and react with NH for 10 h 4 Cl solution was used to quench the reaction, then diluted with 3×10 mL ethyl acetate, extracted, dried with anhydrous sodium sulfate, spin-dried and separated by column chromatography to obtain 0.6 g of the product as a chiral phosphine compound functionalized with binaphthylvinyl groups. body.
[0037] (2) Preparation of functionalized mesoporous silicon materials
[0038]Under argon atmosphere, under argon atmosphere, weigh 200mg of the above-prepared chiral phosphine ligand, 1.0g of mercapto-functionalized SBA-15 and 53mg of AIBN in a flask, a...
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