Tropine alkenyl rare earth metal catalyst, preparation method and application thereof
A technology of metal catalysts and alkenyl rare earths, which is applied in chemical instruments and methods, organic chemistry, and compounds containing elements of group 3/13 of the periodic table, etc. It can solve the problems that have not been reported by anyone, and do not have the ability to adapt to large-scale industrialization processes. Response time-consuming and other issues
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Embodiment 1
[0072] (1) preparation of tropene ligand
[0073]
[0074] First, add 25.0g (177mmol) of tropinol and 12g (11.5mL) of glacial acetic acid into a 250mL eggplant bottle respectively to obtain a mixed solution a, put the eggplant bottle in an ice bath, and add the 46 g (25 mL) of concentrated sulfuric acid was added dropwise to obtain a mixed solution b;
[0075] Next, heat the eggplant bottle containing the mixed solution b to 165°C under an argon atmosphere, take out the eggplant bottle after 22 hours of reaction, cool to 25°C, adjust the pH to 13 with NaOH solution, and obtain a mixed solution containing the target product. solution c;
[0076] Finally, add anhydrous diethyl ether (30ml) to the mixed solution c, separate layers to obtain an aqueous phase and an organic phase, and add anhydrous MgSO 4 After (8g), filter, take the liquid and carry out normal pressure distillation, collect 165~170 ℃ component, pass through a neutral alumina (Brockman Activity I) chromatograp...
Embodiment 2
[0082] (1) preparation of tropene ligand
[0083]
[0084] First, add 25.0g (177mmol) of tropinol and 12g (11.5mL) of glacial acetic acid into a 250mL eggplant bottle respectively to obtain a mixed solution a, put the eggplant bottle in an ice bath, and add the 46 g (25 mL) of concentrated sulfuric acid was added dropwise to obtain a mixed solution b;
[0085] Next, heat the eggplant bottle containing the mixed solution b to 160°C under a nitrogen atmosphere, take out the eggplant bottle after 20 hours of reaction, cool to 20°C, and adjust the pH to 14 with NaOH solution to obtain a mixed solution containing the target product c;
[0086] Finally, add anhydrous diethyl ether (25ml) to the mixed solution c, separate layers to obtain an aqueous phase and an organic phase, and add anhydrous MgSO 4 After (5g), filter, take the liquid and carry out vacuum distillation, collect 80~100 ℃ component, pass through a neutral alumina (Brockman Activity I) chromatographic column after...
Embodiment 3
[0092] (1) preparation of tropene ligand
[0093]
[0094] First, add 25.0g (177mmol) of tropinol and 12g (11.5mL) of glacial acetic acid into a 250mL eggplant bottle respectively to obtain a mixed solution a, put the eggplant bottle in an ice bath, and add the 46 g (25 mL) of concentrated sulfuric acid was added dropwise to obtain a mixed solution b;
[0095] Next, heat the eggplant bottle containing the mixed solution b to 170°C under a nitrogen atmosphere, take out the eggplant bottle after 24 hours of reaction, cool to 22°C, adjust the pH to 13 with NaOH solution, and obtain a mixed solution containing the target product c;
[0096] Finally, add anhydrous diethyl ether (35ml) to the mixed solution c, separate layers to obtain an aqueous phase and an organic phase, and add anhydrous MgSO 4 After (10g), filter, take the liquid and carry out normal pressure distillation, collect 165~170 ℃ component, pass through a neutral alumina (Brockman Activity I) chromatographic col...
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