Preparation method of organic cation-anion pair
An anion, cation, and organic technology, applied in the field of polymer material preparation, can solve the problems of poor solubility, poor reaction repeatability, unfavorable scale-up, etc., and achieve the effect of convenient preparation, simple process, and good solubility
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[0019] The embodiment of the present invention provides a method for preparing an organic anion-cation pair, using a quaternary ammonium base or a quaternary phosphine base to prepare various types of organic anion-cation pairs with a low-cost ion exchange, and the prepared organic anion-cation pairs can be used as The base is used in the metal-catalyzed coupling reaction, and the preparation method specifically includes:
[0020] After the tetraalkyl ammonium hydroxide or phosphine hydroxide aqueous solution is mixed with the acid, the N 2 Stir under protection for 8-12 hours to obtain an ion exchange product, freeze-dry it for 24 hours to obtain a solid-state ion-exchange product, vacuum-dry the solid-state ion-exchange product at a temperature of 30-50°C, and obtain the ion-exchange product after 24 hours Organic anion-cation pairs.
[0021] The organic anion and cation pair prepared above can be used as a base in a metal-catalyzed coupling reaction, and the reaction metho...
Embodiment 1
[0028] This example provides a method for preparing organic anion and cation pairs, which is a method for preparing various types of organic anion and cation pairs with low-cost ion exchange using quaternary ammonium bases or phosphonium bases as raw materials. Organic anion-cation pairs can be used as bases in metal-catalyzed coupling reactions, and the method specifically includes:
[0029] a. After tetraalkyl ammonium hydroxide or phosphine hydroxide and acid are miscible in water, a reaction mixture is obtained;
[0030] b. the resulting reaction mixture was placed under nitrogen N 2 Stirring under protection for 8 to 12 hours to obtain an ion exchange product;
[0031] c. Freeze-drying the obtained ion-exchange product for 24 to 48 hours, and obtaining the ion-exchange product in solid form after freeze-drying;
[0032] d. After vacuum-drying the obtained solid-state ion-exchange product at a temperature of 30-50°C for 24-36 hours, an organic anion-cation pair is obtain...
Embodiment 2
[0042] This embodiment provides a method for preparing an organic anion-cation pair, which specifically includes the following steps:
[0043] a. taking tetraalkylammonium hydroxide or tetraalkylphosphine hydroxide as raw material and equimolar acid in aqueous solution to obtain the first mixture;
[0044] b. Stir with nitrogen protection for 12 hours, the organic ion pair product of ammonium salt cation or phosphonium salt cation and acid radical anion;
[0045] c. After the above-mentioned organic ion pair product is freeze-dried, the organic ion pair product of ammonium salt cation or phosphonium salt cation and acid radical anion in solid form can be obtained;
[0046] d. Dry the organic ion pair product of ammonium salt cation or phosphonium salt cation and acid radical anion in a solid state at 30-50°C for 24 hours in vacuum to obtain an organic anion-cation pair; in practice, the preferred drying temperature is 40°C, The drying time is 24 hours. If the drying time is l...
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