Polyhedral oligomeric silsesquioxane dendritic macromolecule catalyst and application thereof
A technology of polysilsesquioxane and dendrites, which is applied in the field of polyhedral oligomeric silsesquioxane dendrimers to achieve high catalytic activity and enantioselectivity, and improve catalytic efficiency and enantioselectivity Effect
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Embodiment 1
[0042] Embodiment 1: the tetradentate Schiff base B that chloromethylene replaces 1 preparation of
[0043]
[0044] Dissolve (1S,2S)-cyclohexanediamine (21.3g, 142mmol) in absolute ethanol (200mL), cool in an ice bath to 0-5°C, and slowly add anhydrous hydrogen chloride ether solution (14.2g , 142mmol, 36% in ether), the reaction was exothermic and a white precipitate was formed. After the acid addition was complete, the mixture was warmed to room temperature and stirred at room temperature for 12 hours. The precipitate was collected by suction filtration under reduced pressure, washed with excess diethyl ether (100 mL), and dried in vacuum to obtain (1S,2S)-cyclohexanediamine monohydrochloride product in the form of white powder, with a yield of 94%.
[0045] Add (1S,2S)-cyclohexanediamine monohydrochloride (6.0g, 40mmol), 3,5-ditert- Butyl salicylaldehyde (9.35g, 40mmol) and 4A molecular sieves (2.0g), after the reaction mixture was stirred at room temperature for 6 h...
Embodiment 2
[0046] Embodiment 2: [POSS-(Salen-Co II ) 8 ] (Compound D 1 ) preparation
[0047]
[0048] Compound C 1 and D 1 middle:
[0049] The 5-chloromethylene substituted tetradentate Schiff base Salen ligand B 1 (4.32g, 8mmol) and n-Bu 4 NI (295 mg, 0.8 mmol) was dissolved in dichloromethane (150 mL), and compound A {octamercaptopropyl POSS, [Si 8 o 12 (C 3 h 6 SH) 8 ]} (1.02g, 1mmol) and triethylamine (1.1mL, 8mmol), stirred at room temperature for 16 hours. The reaction mixture was washed successively with saturated aqueous sodium bicarbonate solution (40 mL) and saturated saline solution, dried over anhydrous sodium sulfate, filtered and the solvent was removed under reduced pressure. The resulting yellow solid C 1 After washing with n-hexane (80 mL) and a small amount of ether, it was dissolved in dichloromethane (100 mL). Add a methanol solution (60 mL) of 4.0 g (8 mmol) of cobalt acetate tetrahydrate to the above solution, then add dropwise to the above liga...
Embodiment 3
[0050] Embodiment 3: Catalyst [POSS-(Salen-Co-X) 8 ] preparation
[0051]
[0052] General method: compound D in an open container1 (5.5 g, 1 mmol) was dissolved in dichloromethane (100 mL), trifluoromethanesulfonic acid (HOTf, 725 μL, 8.2 mmol) was added, and the mixture was vigorously stirred under air atmosphere for 5 hours. The solvent was removed under reduced pressure, and the obtained solid was washed with n-hexane until the filtrate was colorless. The resulting solid was dissolved in dichloromethane (80mL), filtered to remove insoluble impurities, the solvent was removed under reduced pressure, and dried in vacuo to obtain a brown powder solid [POSS-(Salen-Co-OTf) 8 ], yield 87%. MALDI-TOF MS (calcd for C 296 h 408 co 8 f 24 N 16 o 52 S 16 Si 8 :6681,Found:6704[M+Na] + ). According to the same operation steps, the catalyst [POSS-(Salen-Co-OTs) 8 ] (85% yield) and [POSS-(Salen-Co-OAc) 8 ] (72% yield).
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