Compound and preparation method thereof
A compound, alkenylation technology, applied in chemical instruments and methods, preparation of halogenated hydrocarbons, organic chemistry, etc., can solve the problems of unsuitability for industrial production, complicated synthesis processes, and high production costs, and achieves simple post-processing steps and can be used. Strong controllability and the effect of reducing power consumption
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[0061] According to one embodiment of the present invention, the compound is:
[0062]
[0063] According to one embodiment of the present invention, the compound is:
[0064]
[0065] According to one embodiment of the present invention, the compound is:
[0066]
[0067] According to one embodiment of the present invention, the compound is:
[0068]
[0069] According to one embodiment of the present invention, the compound is:
[0070]
[0071] According to one embodiment of the present invention, the compound is:
[0072]
[0073] According to one embodiment of the present invention, the compound is:
[0074]
[0075] According to one embodiment of the present invention, R 1 Selected from: hydrogen, straight-chain alkyl with 1-10 carbon atoms or straight-chain alkoxy with 1-10 carbon atoms; R 2 Selected from: Hydrogen, Cl, F, CN, OCF 3 、CF 3 ,, SCN, CHF 2 、OCHF 2 , a straight-chain alkyl group with 1-10 carbon atoms or a straight-chain alkoxy ...
Embodiment 1
[0102] according to figure 1 In the flow chart of the preparation method shown, first enter the coupling step S1100: dissolve 1eq reactant 1-a-1 and 1eq reactant 1-b-1 in the solvent, add 1eq sodium bicarbonate, and add the amount of catalyst under nitrogen protection Tetrakis(triphenylphosphine)palladium, heated to reflux and stirred for 2h, then extracted after cooling down to room temperature, and passed through a silica gel column to obtain compound 2-a-1, wherein the solvent was a mixed solvent of toluene, ethanol and water, toluene, ethanol and The volume ratio of water is 1:3:3, and the total volume is adjusted according to the amount of reactant 1-a-1. Generally, 1g of reactant 1-a-1 corresponds to 10ml of solvent. The catalyst is preferably tetrakis(triphenylphosphine) For palladium, toluene is preferred as the extraction agent during extraction, and toluene is preferred for elution through a silica gel column, and the obtained 2-a-1 is a white solid with a yield of 9...
Embodiment 2
[0107] according to figure 1 Show the flow chart of the preparation method, first enter the coupling step S1100: dissolve 1eq reactant 1-a-1 and 1.2eq reactant 1-b-1 in the solvent, add 3eq sodium bicarbonate, and add the catalyst under nitrogen protection A certain amount of tetrakis(triphenylphosphine) palladium was heated to reflux and stirred for 4h, then extracted after cooling down to room temperature, and passed through a silica gel column to obtain compound 2-a-1, wherein the solvent was a mixed solvent of toluene, ethanol and water, toluene, ethanol The volume ratio with water is 4:3:3, and the total volume is adjusted according to the amount of reactant 1-a-1. Generally, 1 gram of reactant 1-a-1 corresponds to 10ml of solvent. The catalyst is preferably tetrakis(triphenyl Phosphine) palladium, toluene is preferably used as the extractant during extraction, and toluene is preferably used for elution through a silica gel column, and the obtained 2-a-1 is a white solid ...
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