Method for purification of indole derivative trimer, electrode active substance and electrochemical cell
A technology of indole derivatives and active materials, applied in electrochemical cells, preparation of electrode active materials, and electrode active materials fields, can solve the problems such as the performance degradation of electrode active materials, and achieve the effect of excellent leakage characteristics
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preparation Embodiment 1
[0074] Preparation Example 1 (preparation of indole derivative trimer)
[0075] In a 200ml three-necked flask, 10ml of acetonitrile was added; and 1.42g of methyl indole-6-carboxylate monomer was dissolved therein. On the other hand, to prepare an oxidizing agent solution, 16.2 g of anhydrous ferric chloride and 5.4 g of water were added and dissolved in 40 ml of acetonitrile, and stirred for 10 minutes. Then, the prepared oxidant solution was added dropwise to the acetonitrile solution of methyl indole-6-carboxylate monomer within 30 minutes, followed by stirring at 60 °C for 10 hours. The reaction solution turned from light yellow to green. The reaction was stopped at this point; the reaction solution was suction filtered, washed with acetonitrile at room temperature, then washed with methanol, and dried in air at 120° C. for 5 hours to obtain 1.12 g of 6,11-dihydro-5H- The green color of trimethyl diindole-[2,3-a:2',3'-c]carbazole-3,8,13-tricarboxylate (methyl indole-6-ca...
Embodiment 1
[0078] About 1 g of the trimer obtained in Preparation Example 1 was transferred to a 200 ml beaker; 15 g of 5% by weight aqueous sulfuric acid was added as a solvent; the mixed solvent was stirred at normal temperature for 5 minutes; Raise to 180°C and hold for 30 minutes. The mixed solvent was mixed with 8 g of 1H-imidazole, and kept stirring at the same temperature for 10 minutes. Subsequently, the trimer was isolated from the solvent by suction filtration; the filtered trimer was washed slightly with boiling water and dried to obtain pale green crystals. The filtrate was yellow.
Embodiment 2
[0080] Example 2 was carried out as in Example 1 except that 20% by weight aqueous sulfuric acid was used as the solvent.
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