Novel spiro aza-carbene metal complex, intermediate, and preparation method and application for novel spiro aza-carbene metal complex
A metal complex, azacarbene technology, applied in the direction of organic compound/hydride/coordination complex catalyst, indium organic compound, platinum group organic compound, etc. High performance, easy operation and high yield
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Embodiment 1
[0036] The preparation method of the novel spirocyclic azacarbene metal complex of the present invention is to use spirocyclic diketone as a raw material, undergo imidization and reduction to obtain a spirocyclic diamine compound, and cyclize it with an orthoformate derivative to form a salt to obtain nitrogen The heterocarbene precursor is then reacted with a metal compound under the action of a base to obtain a spirocyclic azacarbene metal complex.
[0037] Concrete preparation steps are as follows:
[0038] (1) Using spirocyclic diketone as raw material, react with substituted aromatic amine compounds (substituted aniline, substituted naphthylamine or substituted pyridylamine) under the conditions of protonic acid or Lewis acid, and imidize the carbonyl to obtain spirocyclic For bis-imine compounds, the molar ratio of spiro diketone to substituted aromatic amine compounds is 1:2-1:4, and the reaction temperature is 20-50°C. The reaction formula is as follows:
[0039]
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Embodiment 2
[0055] Spirocyclic azacarbene metal complexes Two synthetic routes were adopted, and for the convenience of distinction, the obtained products were recorded as and The synthetic route is as follows:
[0056] (a) Synthetic route
[0057]
[0058] (b) Synthetic route
[0059]
[0060] In the synthetic route, the preparation process of product 3 is as follows: under the protection of argon, aniline (2mL, 22mmol) was dissolved in spiro[4.4]-nonane-1,6-dione 1 (1.5200g, 10mmol) in toluene (100mL ) solution, and then slowly added a dichloromethane solution of titanium tetrachloride (2mol / L, 20mL, 40mmol) under stirring. Then the system was stirred at room temperature for 6 hours, and triethylamine (42 mL, 300 mmol) was slowly added to the system. The above mixture was stirred at 0 °C for 10 min, after which saturated sodium carbonate solution (20 mL) was added. The organic phase was separated, and the aqueous phase was extracted with dichloromethane (50 mL×3). The or...
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