Sulfonium sulfonate salt photoacid generator synthesized from guaiacol and synthesis method for sulfonium sulfonate salt photoacid generator
A technology of photoacid generator and guaiac alcohol, which is applied in the preparation of sulfonate, photosensitive materials used in photomechanical equipment, organic chemistry, etc., can solve the problems of inability to reduce edge roughness, etc., and achieve easy preparation, generation, Effect of reducing line width roughness and increasing fat solubility
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Embodiment 1
[0040] This embodiment provides a kind of sulfonate salt photoacid generator synthesized by guaiacol, the reaction scheme of the synthetic method of this photoacid generator is as follows:
[0041]
[0042] It specifically includes the following steps:
[0043] S1. Sodium hydroxide (7g, 175mmol) was dissolved in water (17g) to form a 30% sodium hydroxide solution; methyl fluorosulfonyl difluoroacetate 1-1 (10g, 52mmol) was added to ice water ( 33g) to obtain the reaction solution, and slowly add 30% sodium hydroxide solution prepared under stirring into the above-mentioned reaction solution, after the addition, the reaction solution was stirred in an ice bath (control temperature is lower than 10 degrees Celsius) 2.5 hours, then continue to stir at room temperature for 1 hour, start heating, make the temperature rise to 95 degrees Celsius within 30 minutes, and stir at 95 degrees Celsius for 3 hours, stop heating, cool to room temperature, neutralize with hydrochloric acid,...
Embodiment 2
[0048] This embodiment provides a kind of sulfonate salt photoacid generator synthesized by guaiacol, the reaction scheme of the synthetic method of this photoacid generator is as follows:
[0049]
[0050] It specifically includes the following steps:
[0051] S1. Under the protection of nitrogen at 0°C, add pyridine (9g, 114mmol), bis(trichloromethyl)carbonate (4.5g, 15mmol) into dichloromethane (300g), and slowly add heal Chuang wood alcohol 2-1 (10g, 45mmol) to obtain the reaction solution; then, the reaction solution was stirred at room temperature for 3 hours, and then 1,1-difluoro-2-hydroxyl-ethanesulfonic acid sodium salt (8.8g , 48mmol) was added in the reaction solution, stirred for 10 hours, the reaction solution was concentrated under vacuum to obtain a mixture, the mixture was filtered to obtain a solid, and the solid was washed three times with acetonitrile (150g×3), the acetonitrile solution was collected, and the acetonitrile solution collected was concentra...
Embodiment 3
[0054] This embodiment provides a kind of sulfonate salt photoacid generator synthesized by guaiacol, the reaction scheme of the synthetic method of this photoacid generator is as follows:
[0055]
[0056] It specifically includes the following steps:
[0057] S1. Under nitrogen at 0°C, sodium hydride (1.3g, 54mmol) was slowly added to a mixture of guaiacol 3-1 (10g, 45mmol) and anhydrous tetrahydrofuran (200g), and stirred for 20 minutes; Next, ethyl bromoacetate (8 g, 48 mmol) was added dropwise to the above mixture, and stirred for 20 minutes; then, stirred at 25° C. for 6 hours for reaction, and quenched by adding water at 0° C. after the reaction was completed. Concentrate the quenched mixture by rotary evaporation, extract three times with dichloromethane (150g×3), combine the extracts, wash and separate the liquids with saturated brine (100g), dry over anhydrous sodium sulfate, and concentrate by rotary evaporation to obtain Crude product; the crude product was pur...
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