Bridged beta-pyridyl enol tetra-zinc complex, synthesis method and application
A technology of pyridine enol and zinc complexes, applied in the direction of zinc organic compounds, can solve problems such as long cycle, and achieve the effect of broadening the scope of application
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Embodiment 1
[0030] 1. Synthesis of 1-(pyridin-2-yl)-2-acetone ligand
[0031]
[0032]Under a nitrogen atmosphere, 2-picoline (2.79 g, 30 mmol) was added into the reaction flask, and 30 mL of tetrahydrofuran was added to dissolve it. At -10°C, 12.4mL (2.5M, 30mmol) of n-butyllithium was added dropwise, and after half an hour of reaction, the temperature was raised to 25°C for 4h to obtain a dark red solution.
[0033] Under a nitrogen atmosphere, at -5°C, acetonitrile (1.61 mL, 31 mmol) was taken with a syringe and added dropwise to the solution in the previous reaction flask. After half an hour of reaction, the temperature was raised to 27°C and stirred for two days to obtain a brown liquid.
[0034] At -5°C, add 60wt% sulfuric acid solution to the brown liquid obtained from the reaction for acid hydrolysis, until the pH reaches 1, react for 24 hours, and the color of the solution turns dark brown. At -7°C, add saturated sodium hydroxide And excess sulfuric acid solution, dissolve th...
Embodiment 2
[0045] 1. Synthesis of 1-(pyridin-2-yl)-2-acetone ligand
[0046] Under a nitrogen atmosphere, 2-picoline (0.93 g, 10 mmol) was added into the reaction flask, and 10 mL of tetrahydrofuran was added to dissolve it. At -3°C, 4.1mL (2.5M, 10mmol) of n-butyllithium was added dropwise, reacted for half an hour, and then heated to 29°C for 6h to obtain a dark red solution.
[0047] Under nitrogen atmosphere, at -10°C, acetonitrile (0.56mL, 11mmol) was taken with a syringe and added dropwise to the solution in the reaction flask of the previous step. After reacting for half an hour, the temperature was raised to 29°C and stirred for one day to obtain a brown liquid.
[0048] At -5°C, add 65wt% sulfuric acid solution to the brown liquid obtained from the reaction for acid hydrolysis, until the pH reaches 1, react for 36 hours, and the color of the solution turns dark brown. At -10°C, add saturated sodium hydroxide to neutralize the excess sulfuric acid solution, dissolve the resultin...
Embodiment 3
[0056] 1. Synthesis of 1-(pyridin-2-yl)-2-acetone ligand
[0057] Under a nitrogen atmosphere, 2-picoline (1.86 g, 20 mmol) was added into the reaction flask, and 10 mL of tetrahydrofuran was added to dissolve it. At -10°C, 8.2mL (2.5M, 20mmol) of n-butyllithium was added dropwise, reacted for half an hour and then heated to 30°C for 5h to obtain a dark red solution.
[0058] Under nitrogen atmosphere, at -10°C, acetonitrile (1.02mL, 21mmol) was taken by syringe and added dropwise to the solution in the reaction bottle of the previous step. After reacting for half an hour, the temperature was raised to 25°C and stirred for 1.5 days to obtain a brown liquid.
[0059] At -5°C, add 70wt% sulfuric acid solution to the brown solution obtained from the reaction for acid hydrolysis, until the pH reaches 2, react for 36 hours, and the color of the solution turns dark brown. At -0°C, add saturated sodium hydroxide and excess sulfuric acid solution, dissolve the resulting solid with a ...
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