Fluorine-containing diketopyrrolopyrrole quaternary ammonium salt compound and its preparation method and application
A technology of fluorine-containing diketopyrrolopyrrole and diketopyrrolopyrrole, which is applied in the field of fluorine-containing diketopyrrolopyrrole quaternary ammonium salts and its preparation, and can solve the problems of increasing brittleness and stress of the coating
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Embodiment 1
[0056] The preparation method of compound I-1 is as follows:
[0057]
[0058] (1) Preparation of intermediate 3-1
[0059] Add 100ml of tert-amyl alcohol into a 250ml three-neck flask, then cut 4g of sodium into sodium particles and add it, and then add ferric chloride with a catalytic amount of 20-40mg as a catalyst. Heat to 100~105°C, react for 2~3h. Cool down to 50-60°C, add 68.6mmol of compound 2-1, then heat to 100-105°C, add 8ml of diisopropyl succinate compound 1 and 40ml of tert-amyl alcohol into the three-necked flask with a constant pressure dropping funnel , 3 ~ 5s / d, 2-3h drop. Finally, react for another 4 hours, stop the reaction, pour the reaction product into a beaker, add 100ml of methanol to dilute, then add acetic acid to adjust the pH to 7, filter with suction, wash the filter cake with methanol, take the filter cake, heat and dry it, and then use N, N-dimethylformamide was dissolved in heat, cooled and suction filtered, the filter cake was washed wit...
Embodiment 2
[0069] Compound I-2
[0070]
[0071] (1) Preparation of intermediate 3-2
[0072] Add 100ml of tert-amyl alcohol into a 250ml three-necked flask, then cut 4g of sodium into sodium particles and add it, and then add a catalytic amount of 20-40mg of ferric chloride as a catalyst. Heat to 100~105°C, react for 2~3h. Cool down to 50-60°C, add 68.6mmol of compound 2-2, and then heat to 100-105°C. Add 8ml of diisopropyl succinate compound 1 and 40ml of tert-amyl alcohol mixture into a three-necked flask with a constant pressure dropping funnel, drop it in 3-5s / d, 2-3h. Finally, react for another 4 hours, stop the reaction, pour the reaction product into a beaker, add 100ml of methanol to dilute, then add acetic acid to adjust the pH to 7, filter with suction, wash the filter cake with methanol, take the filter cake, heat and dry it, and then use N, N-dimethylformamide was dissolved in heat, cooled and suction filtered, the filter cake was washed with water and methanol in sequ...
Embodiment 3
[0082] Preparation of Compound I-3
[0083]
[0084] (1) Preparation of intermediate 3-3
[0085] Add 100ml of tert-amyl alcohol into a 250ml three-necked flask, then cut 4g of sodium into sodium particles and add it, and then add a catalytic amount of 20-40mg of ferric chloride as a catalyst. Heat to 100~105°C, react for 2~3h. Cool down to 50-60°C, add 68.6mmol of compound 2-3, and then heat to 100-105°C. Add 8ml of diisopropyl succinate compound 1 and 40ml of tert-amyl alcohol mixture into a three-necked flask with a constant pressure dropping funnel, drop it in 3-5s / d, 2-3h. Finally, react for another 4 hours, stop the reaction, pour the reaction product into a beaker, add 100ml of methanol to dilute, then add acetic acid to adjust the pH to 7, filter with suction, wash the filter cake with methanol, take the filter cake, heat and dry it, and then use N, N-dimethylformamide was dissolved in heat, cooled and suction filtered, the filter cake was washed with water and met...
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