Fluoride-free photoacid generator and preparation method thereof
A technology of photoacid generators and cations, which is applied in the preparation of carboxylic acid nitriles, photomechanical equipment, chemical instruments and methods, etc., can solve the problem of uneven distribution of PAG in photoresist films and low surface energy of fluorinated chains , uneven distribution and other problems, to achieve the effect of reducing impact, mild conditions and convenient operation
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Embodiment 1
[0032] The synthetic route of photoacid generator 1-4 is as follows:
[0033]
[0034] Preparation of Intermediate 1-2:
[0035] Dissolve phenylglyoxal hydrate 1-1 (5 g, 32.9 mmol) and malononitrile (2.2, 33.3 mmol) in isopropanol (50 mL), and add 2-bromomalononitrile (4.8 g, 33.1 mmol) with stirring ). Then stir for 30 minutes. Then the reaction solution was filtered to obtain a filter cake. The filter cake was washed and dried with isopropanol to obtain intermediate 1-2 (6.2 g, 25.2 mmol, molar yield 76.6%).
[0036] Preparation of Intermediates 1-3:
[0037] Under stirring condition, sodium acetate (2g, 24.4mmol) was dissolved in water (10mL), then added to a solution of intermediate 1-2 (6g, 24.4mmol) in acetonitrile (25mL), and reacted for 2 hours. The reaction solution was evaporated to dryness, the obtained solid was washed with dichloromethane, recrystallized with a mixed solution of isopropanol and water (1:1 by volume), filtered and dried to obtain intermedia...
Embodiment 2
[0041] The synthetic route of photoacid generator 2-4 is as follows:
[0042]
[0043] Preparation of Intermediate 2-2:
[0044] 1-Naphthylglyoxal hydrate 2-1 (5g, 24.7mmol) and malononitrile (1.7, 25.7mmol) were dissolved in isopropanol (50mL), and 2-bromomalononitrile (3.6g , 24.8 mmol). Then stir for 30 minutes. Then the reaction solution was filtered to obtain a filter cake. The filter cake was washed and dried with isopropanol to obtain intermediate 2-2 (5.7 g, 19.2 mmol, molar yield 77.8%).
[0045] Preparation of Intermediate 2-3:
[0046] Under stirring conditions, sodium acetate (1.6g, 19.5mmol) was dissolved in water (10mL), and then added to a solution of acetonitrile (25mL) containing intermediate 2-2 (5.7g, 19.2mmol), reaction 2 Hour. The reaction solution was evaporated to dryness, the obtained solid was washed with dichloromethane, recrystallized with a mixed solution of isopropanol and water (1:1 by volume), filtered and dried to obtain intermediate 2-...
Embodiment 3
[0050] The synthetic route of photoacid generator 3-4 is as follows:
[0051]
[0052] Preparation of intermediate 3-2:
[0053] Dissolve 3,4-dimethoxyphenylglyoxal hydrate 3-1 (5 g, 23.6 mmol) and malononitrile (1.6, 24.2 mmol) in isopropanol (50 mL), and add 2-bromo Malononitrile (3.5 g, 24.1 mmol). Then stir for 30 minutes. Then the reaction solution was filtered to obtain a filter cake. The filter cake was washed and dried with isopropanol to obtain intermediate 3-2 (5.5 g, 18.0 mmol, molar yield 76.2%).
[0054] Preparation of intermediate 3-3:
[0055] Under stirring condition, sodium acetate (1.5g, 18.3mmol) was dissolved in water (10mL), then was added to the solution containing intermediate 3-2 (5.5g, 18.0mmol) in acetonitrile (25mL), reaction 2 Hour. The reaction solution was evaporated to dryness, the obtained solid was washed with dichloromethane, recrystallized with a mixed solution of isopropanol and water (1:1 by volume), filtered and dried to obtain in...
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