Economic and efficient method for asymmetric synthesis of R-configuration aromatic alcohol through copper salt catalysis
A technology for asymmetric and aromatic alcohols, which is applied in the field of catalytic asymmetric hydrosilylation to prepare optically active alcohols, can solve the problems of limited wide application and low stability, and achieve easy availability of raw materials, high yield and enantioselectivity, and reaction The effect of mild conditions
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Embodiment 1
[0012] At room temperature, 0.006g of catalyst precursor Cu(OAc) 2 ·H 2 O. 0.003g chiral bisphosphine ligand (R)-BINAP was stirred and mixed with 3mL toluene for coordination reaction for 0.5h; 180μL polymethylhydrogensiloxane was added dropwise, and stirring was continued for 30min to generate catalytically active substances in situ; Add 117 μL of substrate acetophenone, react at 55°C for 4 hours, and monitor the reaction by thin-layer chromatography; after the reaction, add methanol and sodium hydroxide solution, stir vigorously, and obtain a mixture of chiral aromatic alcohol crude products after hydrolysis.
[0013] The mixed solution obtained after hydrolysis was extracted and separated with dichloromethane, and the organic layer was collected. The organic layer was washed with water and dried over anhydrous sodium sulfate. After drying, the solvent was distilled off under reduced pressure to obtain a crude product concentrate, which was further separated and purified b...
Embodiment 2
[0015] At room temperature, 0.006g of catalyst precursor Cu(OAc) 2 ·H 2 O. 0.006g chiral bisphosphine ligand (R)-BINAP was stirred and mixed with 3mL toluene for coordination reaction for 1h; 180μL polymethylhydrogensiloxane was added dropwise, and stirring was continued for 30min to generate catalytically active substances in situ; 130 μL of the substrate 2-chloroacetophenone was placed at 25°C for 4 hours, and the reaction was monitored by thin-layer chromatography; after the reaction was completed, methanol and sodium hydroxide solution were added, vigorously stirred, and a mixture of crude chiral aromatic alcohols was obtained after hydrolysis .
[0016] The mixed solution obtained after hydrolysis was extracted and separated with dichloromethane, and the organic layer was collected. The organic layer was washed with water and dried over anhydrous sodium sulfate. After drying, the solvent was distilled off under reduced pressure to obtain a crude product concentrate, wh...
Embodiment 3
[0018] At room temperature, 0.002g catalyst precursor Cu(OAc) 2 ·H 2O. 0.010g chiral bisphosphine ligand (R)-BINAP was stirred and mixed with 3mL dihydrofuran for coordination reaction for 1h; 570μL triethoxysilane was added dropwise, and stirring was continued for 30min to generate catalytically active substances in situ; 130 μL of the substrate 4-chloroacetophenone, reacted at 25°C for 10 hours, and monitored the reaction by thin-layer chromatography; after the reaction, add methanol and sodium hydroxide solution, stir vigorously, and obtain a mixture of chiral aromatic alcohol crude products after hydrolysis .
[0019] The mixed solution obtained after hydrolysis was extracted and separated with dichloromethane, and the organic layer was collected. The organic layer was washed with water and dried over anhydrous sodium sulfate. After drying, the solvent was distilled off under reduced pressure to obtain a crude product concentrate, which was further separated and purifie...
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