Tetracarboxylic dianhydride and preparation method thereof
A technology of tetracarboxylic dianhydride and chemical formula, which is applied in the field of tetracarboxylic dianhydride and its preparation, and can solve problems such as lack of processability
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[0117] A method of preparing tetracarboxylic dianhydride according to an exemplary embodiment of the present invention may be shown in Reaction Formula 1 below, but of course various modifications may be made by a general organic synthesis method.
[0118] [Reaction 1]
[0119]
[0120] Furthermore, another exemplary embodiment of the present invention is the use of tetracarboxylic dianhydride, and specific embodiments thereof will be described later.
[0121] The first embodiment of the present invention may be a composition including tetracarboxylic dianhydride represented by Chemical Formula 1.
[0122] The second embodiment of the present invention may be a polyimide precursor solution including a polyimide precursor derived from tetracarboxylic dianhydride represented by Chemical Formula 1. Referring to FIG. Specifically, the polyimide precursor may be a polyamic acid obtained through a polymerization reaction including tetracarboxylic dianhydride represented by Chemi...
Embodiment 1
[0233]
[0234] Step 1. Substance A
[0235] In a nitrogen atmosphere, 3,4-dimethylphenylboronic acid (7.95g, 53.0mmol), 1,2-dibromo-4,5-xylene (14g, 53.0mmol), triphenylphosphine (0.42 g, 1.59mmol) and K 2 CO 3 (21.9g, 159mmol) was added to a mixed solution of 100ml degassed water and 70ml tetrahydrofuran (THF). Raise the temperature to 80°C, add Pd(PPh 3 ) 4 (0.61 g, 0.53 mmol), stirred for 30 hours. The temperature was lowered to room temperature, and the organic solvent was removed by distillation under reduced pressure, 100ml of dichloromethane (DCM) and 50ml of water were added, the organic layer was washed with water, and washed with anhydrous MgSO 4 Remove moisture. Filter out MgSO 4 Afterwards, the solvent was removed and the material was isolated by column chromatography to afford material A in 75% yield.
[0236] HRMS (EI, m / z): [M+]C 16 h 13 Br, calculated 288.05; found 269.16.
[0237] 1 H-NMR (ppm, CDCl 3 ): 7.44 (1H, s), 7.15-7.20 (3H, m), 7.10 (...
Embodiment 2
[0263]
[0264] Step 1. Substance G
[0265] Substance A (5.0 g, 17.47 mmol) was dissolved in 100 ml of anhydrous tetrahydrofuran (THF), the temperature was lowered to -78 °C, and n-butyllithium (7.6 ml of a 2.5M solution in hexane, 18.8 mmol). After stirring for 1 hour, 9H-thioxanth-9-one (3.375 g, 15.9 mmol) was added to the reactant, and stirred for 12 hours while raising the temperature to room temperature. 100ml of water was added, the solvent was removed under reduced pressure, and 100ml of dichloromethane (DCM) was added to extract the organic matter. with anhydrous MgSO 4 The water was removed, the solvent was removed by filtration, and the resulting material was added to 50 ml of acetic acid at 0°C. 1 ml of 35% by weight hydrochloric acid was added, heated to reflux for 4 hours, and then stirred at room temperature for 1 hour. The reaction was poured into 200 ml of water and the resulting solid was filtered, precipitated with MeOH and stirred to obtain substanc...
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