Catalyst for olefin hydrosilylation reaction, its preparation method and olefin hydrosilylation reaction using the catalyst
A technology for hydrosilylation reaction and hydrosilylation, which is used in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc. The preparation method is simple and fast, with good stability and the effect of improving selectivity
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[0035] A preparation method for a catalyst for olefin hydrosilylation reaction, comprising the following steps:
[0036] (1) With polyethylene glycol having an average molecular weight of 200, 300, 400, 600, and respectively with thionyl chloride and imidazole as raw materials, four kinds of terminal imidazole polyethylene glycols of A, B, C, and D are prepared, The structural formula is:
[0037]
[0038] The four end-group imidazole polyethylene glycols of A, B, C and D, n=4 in A, n=6 in B, n=8 in C, n=12 in D;
[0039] The preparation method is carried out according to the method in the document New J.Chem., 2013,37,269;
[0040] (2) Add the above-mentioned four kinds of end-group imidazole polyethylene glycols A, B, C, D and 1-chlorocarboxylic acid respectively according to the molar ratio of 1:2 into a tank with magnetic stirring, heating device and condensing device In a reaction vessel, and use trichloroethane as the reaction solvent, stir and react for 12 hours at...
Embodiment 1
[0051] In a 100 ml three-neck flask, add 3.38 g of imidazolyl polyethylene glycol A, 1.88 g of chloroacetic acid, and 30 ml of trichloroethane, raise the temperature to 80° C., stir the reaction for 12 h, and cool to room temperature. Trichloroethane was removed by decantation, washed with ethyl acetate (25 mL×2), and the residual solvent was removed under reduced pressure. Solid is dissolved with 50 milliliters of absolute ethanol, adds 1.98g di-tert-butoxyferrous iron Fe(O t Bu) 2 , stirred at 50°C for 3h, removed ethanol by rotary evaporation, and dried in a vacuum oven at 70°C for 24h. The obtained solid was suspended in 25 ml of anhydrous tetrahydrofuran, 2.24 g of potassium tert-butyl alkoxide was added, stirred for 30 minutes, 39 g of Karstedt catalyst with a platinum content of 10% was added, stirred for 1 h, and the solvent was removed to obtain a metal carboxylate cyclized polyether- N-Heterocyclic Carbene Platinum Complex Integrated Catalyst.
[0052]Take 0.1 mmo...
Embodiment 2
[0055] Take 0.1 mmol of the catalyst of Example 1, 1 mol of 1-hexene and 1.1 mol of triethoxyhydrogensilane in a closed container containing a magnetic stirrer, react in a silicone oil bath at 80°C for 4 hours, and the conversion of 1-hexene is 99.3%, β-addition product selectivity is 99.4%.
[0056] Separate the upper layer product, add another 1mol 1-hexene and 1.1mol triethoxyhydrogensilane, react under the same conditions for 4h, the conversion rate of 1-hexene is 99.0%, and the selectivity of β-addition product is 99.7%.
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