Tetrakis(ethylmethylamino)hafnium synthesis method
A synthetic method, ethylamino technology, applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., can solve problems such as increasing operation difficulty and cost, reducing reaction efficiency, and difficulty in filtration and separation , to achieve the effect of saving reaction cost, simple operation and cost reduction
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Embodiment 1
[0024] Embodiment 1: the synthesis of hafnium tetramethylethylamino
[0025] (1) Under an inert atmosphere, add 130 g of methylethylamine and 600 mL of n-hexane into a 2000 mL three-necked flask, stir mechanically, and place the reaction flask at -10°C. Add 800 mL of 2.5 mol / L n-butyllithium in n-hexane solution dropwise into the reaction flask. After the dropwise addition, the reaction was stirred for 5 hours.
[0026] (2) Add 160 grams of hafnium tetrachloride into the above reaction system, and keep the temperature of the reaction system not higher than 60°C. After adding hafnium tetrachloride, let the reaction system react for 18 hours under the condition of mechanical stirring and inert gas protection.
[0027] (3) After the reaction is over, change the reaction device directly into a distillation device, remove the reaction solvent under normal pressure, wait for the solvent n-hexane to be completely removed, distill under reduced pressure, and collect the fraction at ...
Embodiment 2
[0028] Embodiment 2: the synthesis of hafnium tetramethylethylamino
[0029] (1) Under an inert atmosphere, add 236 g of methylethylamine and 500 mL of n-hexane into a 2000 mL three-necked bottle, stir mechanically, and place the reaction bottle at -50 °C. Add 800 mL of 2.5 mol / L n-butyllithium in n-hexane solution dropwise into the reaction flask. After the dropwise addition, the reaction was stirred for 12 hours.
[0030] (2) Add 160 grams of hafnium tetrachloride into the above reaction system, and keep the temperature of the reaction system not higher than 60°C. After adding the hafnium tetrachloride, let the reaction system react for 30 hours under the condition of mechanical stirring and inert gas protection.
[0031] (3) After the reaction is over, change the reaction device directly into a distillation device, remove the reaction solvent under normal pressure, wait for the solvent n-hexane to be completely removed, distill under reduced pressure, and collect the frac...
Embodiment 3
[0032] Embodiment 3: the synthesis of tetramethylethylamino hafnium
[0033] (1) Under an inert atmosphere, add 177 g of methylethylamine and 700 mL of n-hexane into a 2000 mL three-necked bottle, stir mechanically, and place the reaction bottle at -80 °C. Add 800 mL of 2.5 mol / L n-butyllithium in n-hexane solution dropwise into the reaction flask. After the dropwise addition, the reaction was stirred for 10 hours.
[0034] (2) Add 160 grams of hafnium tetrachloride into the above reaction system, and keep the temperature of the reaction system not higher than 60°C. After adding hafnium tetrachloride, let the reaction system react for 20 hours under the condition of mechanical stirring and inert gas protection.
[0035](3) After the reaction is over, change the reaction device directly into a distillation device, remove the reaction solvent under normal pressure, wait for the solvent n-hexane to be completely removed, distill under reduced pressure, and collect the fraction ...
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