Dicyanovinyl substituted quinacridone derivatives with alcohol/water solubility and applications thereof
A water-soluble, dicyandiamide technology, applied in organic chemistry, semiconductor/solid-state device manufacturing, electrical solid-state devices, etc., can solve problems such as unsuitability and unfavorable device stability
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Embodiment 1
[0020] Example 1: Compound DCNQA-C 4 -Synthesis of Br:
[0021]
[0022] Put quinacridone (3.12g, 10mmol), 1,4-dibromobutane (10.8g, 50mmol), sodium hydride (1.43g, 50mmol), and 50mL dry tetrahydrofuran into a 100 three-necked flask, and heat to reflux for 24 hours , cooled to room temperature, added 50mL of methanol to neutralize the remaining sodium hydride, added 200mL of water and 500mL of dichloromethane to separate the liquid, and spin-dried the organic solvent to obtain a solid that was recrystallized with chloroform / petroleum ether to obtain the red product QA-C 4 -Br2.91g, yield 62.5%, put into next step directly.
[0023]The QA-C synthesized in the previous step 4 -Br (2.91g, 5.0mmol), malononitrile (0.66g, 10.0mmol), 500mL of anhydrous and dry dichloromethane were placed in a 1L two-necked bottle, and TiCl was slowly added dropwise in sequence 4 (28.50g, 150.0mmol) , Dried pyridine (63.20g, 800.0mmol), after the dropwise addition, the system was stirred at ro...
Embodiment 2
[0024] Example 2: Compound DCNQA-C 5 -Synthesis of Br:
[0025]
[0026] QA-C 5 -Synthetic method of Br and QA-C 4 -Br is exactly the same, except that 1,5-dibromopentane is used as starting material instead of 1,4-dibromobutane (yield 60.2%).
[0027] DCNQA-C 5 -The second step synthesis of Br and DCNQA-C 4 -Br method is exactly the same, just use QA-C 5 -Br as starting material (dark green solid, 72.2% yield). The molecular ion mass determined by mass spectrometry is: 704.5 (calculated value: 704.1); theoretical element content (%) C 36 h 30 Br 2 N 6 : C, 61.31; H, 4.30; N, 11.72; Measured element content (%): C, 61.20; H, 4.28; N, 11.90. The above analysis results indicated that the obtained product was the expected product.
Embodiment 3
[0028] Example 3: Compound DCNQA-C 6 -Synthesis of Br:
[0029]
[0030] QA-C 6 -Synthetic method of Br and QA-C 4 -Br is exactly the same, except that 1,6-dibromohexane is used as starting material instead of 1,4-dibromobutane (65.9% yield).
[0031] DCNQA-C 6 -The second step synthesis of Br and DCNQA-C 4 -Br method is exactly the same, just use QA-C 6 -Br as starting material (dark green solid, 75.1% yield). The molecular ion mass determined by mass spectrometry is: 732.5 (calculated value: 732.1); theoretical element content (%) C 38 h 34 Br 2 N 6 : C, 62.14; H, 4.76; N, 11.44; Measured element content (%): C, 62.29; H, 4.70; N, 11.37. The above analysis results indicated that the obtained product was the expected product.
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