Synthesis method of functionalized organic phosphine ligand polymer monomer
A technology of a ligand polymer and a synthesis method, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem that temperature-controlled organic phosphine ligands are expensive and difficult to achieve large-scale Production applications, etc.
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[0044] In a specific embodiment, the synthetic method of the functionalized organophosphine ligand polymer monomer provided by the present invention comprises the following steps:
[0045] First, under an ice-water bath and a nitrogen atmosphere, in a three-neck round-bottomed flask with a magnetic stirring bar, sequentially add magnesium powder and anhydrous ether, wherein the weight ratio of magnesium powder / anhydrous ether is 0.001 to 0.5, preferably The weight ratio of magnesium powder / anhydrous ether is 0.005-0.1. The resulting reaction mixture is stirred under these conditions for 0.50-100 hours, preferably 2-50 hours.
[0046] Next, add the mixed solution of p-bromostyrene and anhydrous ether dropwise, wherein the weight ratio of p-bromostyrene / anhydrous ether is 0.01~25, and the preferred weight ratio of p-bromostyrene / anhydrous ether is 0.05~20 . The obtained reaction mixture is stirred under this condition for 0.5-100 hours, preferably the stirring time is 2-50 hou...
Embodiment 1
[0057] In an ice-water bath and a nitrogen atmosphere, in a 100mL three-necked round-bottomed flask with a magnetic stirrer, 0.5g of magnesium powder (Aladdin Reagent Co., Ltd.), 10mL of anhydrous ether (Sinopharm Chemical Reagent Co., Ltd.) were added successively, and the obtained The reaction mixture was stirred under these conditions for 2 hours; then a mixed solution of 4g p-bromostyrene (Aladdin Reagent Co., Ltd.) and 10mL of anhydrous ether was added dropwise, and the resulting reaction mixture was stirred under these conditions for 2 hours; A mixed solution of 6g of phosphorus trichloride (Aladdin Reagent Co., Ltd.) and 10mL of anhydrous ether, the resulting reaction mixture was stirred for 2 hours under these conditions; then 10mL of water was added and stirred for 1 hour, and then the reaction was extracted 3 times with 90mL of ether solution The mixture was combined with the ether extracts, filtered and then rotary evaporated to remove the anhydrous solvent, and the ...
Embodiment 2
[0059] In addition to replacing 0.5g magnesium powder with 0.4g magnesium powder, 3g p-bromostyrene instead of 4g p-bromostyrene and 6g phenylphosphine dichloride (Aladdin Reagent Co., Ltd.) instead of 6g phosphorus trichloride, its operation steps are the same as Example 1 is the same. A light yellow powdery solid was obtained with a yield of 25%, Figure 4 It is a schematic diagram of the technical route for the synthesis of bis(4-vinylphenyl)phenylphosphine ligand polymer monomers according to Example 2. The structure and purity of the obtained product were analyzed by nuclear magnetic resonance spectrum as described in Example 1 above, and it was confirmed that the obtained product was a bis(4-vinylphenyl)ylphenylphosphine ligand polymer monomer.
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