A kind of monophosphine-containing porous organic polymer in-situ encapsulated rhodium catalytic material and its preparation method and application
A polymer and rhodium-catalyzed technology, which is applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, organic silicon compounds, etc., can solve the problems of high operating costs and complex catalyst preparation processes, and achieve the goal of preparing easy effect
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[0043] The invention provides a method for preparing a monophosphine-containing porous organic polymer in-situ encapsulating rhodium catalytic material, comprising the following steps:
[0044] Under an inert gas atmosphere, the carbonyl-functionalized monophosphine ligand, the active metal rhodium, the acidic catalyst and the first organic solvent are mixed to obtain a mixed system;
[0045] The hydrazine hydrate and the second organic solvent are mixed and added dropwise into the mixed system to carry out a polymerization reaction to obtain the monophosphine-containing porous organic polymer in-situ encapsulated rhodium catalytic material.
[0046] In the present invention, unless otherwise specified, the raw materials used are all commercially available products in the field or prepared according to conventional means in the field.
[0047] In the present invention, the carbonyl-functionalized monophosphine ligand (carbonyl-functionalized PPh 3 Ligand monomer), the active ...
Embodiment 1
[0080] Carbonyl functionalized PPh 3 Ligand monomer ( figure 1 Preparation of L1) in: add 15 g of 4-bromobenzaldehyde dimethyl acetal (66 mmol) and 8 volumes of anhydrous tetrahydrofuran under an inert atmosphere, and slowly dropwise add 28 mL of butyllithium (2.5 M at -78 °C) ), continue to stir for 1.0h, 1.37g of phosphorus trichloride is dissolved in 8 times the volume of tetrahydrofuran solution, and then slowly added dropwise to the reaction system, fully reacted for 1.0h, and an equal volume of 2N HCl / THF (1:1) solution is added Continue to react. After the reaction, after quenching, extraction and spin drying, 5.0 g of white solid product was obtained after passing through the column with the eluent of 5:1 petroleum ether:ethyl acetate, with a yield of 72%. Figures 2 to 4 are the prepared carbonyl-functionalized PPh, respectively 3 Ligand Monomer NMR 1 H. 13 C and 31 P spectrum.
[0081] Preparation of monophosphine-containing porous organic polymer in-situ enca...
Embodiment 2
[0083] In Example 2, in addition to weighing 3.88g figure 1 L2 in the monophosphine ligand monomer instead of 3.46g figure 1 Except for the L1 monophosphine ligand monomer in , the rest of the implementation process is the same as that in Example 1. The obtained monophosphine-containing porous organic polymer in-situ encapsulated rhodium catalytic material is designated as catalyst B.
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