Sulfonium sulfonate salt photoacid generator synthesized from cedrol and synthesis method for sulfonium sulfonate salt photoacid generator
The technology of a photoacid generator and a synthesis method is applied in the preparation of sulfonates, photosensitive materials for optomechanical equipment, organic chemistry, etc., which can solve the problems such as the inability to reduce edge roughness, and achieve easy preparation and generation, good transparency. , Improve the effect of edge roughness
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Embodiment 1
[0040] This embodiment provides a kind of sulfonate sulfonium salt photoacid generator synthesized by cederyl alcohol, 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 (18g) to form a solution; methyl fluorosulfonyl difluoroacetate (10g, 52mmol) was added to ice water (25g) to obtain a reaction solution, and Slowly add the prepared sodium hydroxide solution to the above reaction solution under stirring. After the addition, the reaction solution is stirred in an ice bath (control temperature below 10 degrees Celsius) for 2.5 hours, and then continue to stir at room temperature for 1 hour. , start heating, make the temperature rise to 95 degrees Celsius in 30 minutes, and stir at 95 degrees Celsius for 3 hours, stop heating, cool to room temperature, neutralize with hydrochloric acid, filter the reaction solut...
Embodiment 2
[0048] This embodiment provides a kind of sulfonate sulfonium salt photoacid generator synthesized by cederyl alcohol, 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 (9.5g, 120mmol), bis(trichloromethyl)carbonate (5.0g, 17mmol) into dichloromethane (300g), and slowly add it under stirring Cedaryl alcohol 2-1 (10.0g, 45mmol) to obtain a 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 to the reaction solution, stirred for 10 hours, the reaction solution was concentrated under vacuum to obtain a mixture, and n-heptane (120g) was added, and a solid was obtained by filtration. The solid was added to acetonitrile (120g), stirred and dissolved, and the filtrate was collected by fi...
Embodiment 3
[0054] This embodiment provides a kind of sulfonate sulfonium salt photoacid generator synthesized by cederyl alcohol, 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 (1.2g, 50mmol) was slowly added to a mixture of cedaryl alcohol 3-1 (10g, 45mmol) and anhydrous tetrahydrofuran (200g), and stirred for 20 minutes; then, 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. The quenched mixed solution was concentrated by rotary evaporation, extracted three times with dichloromethane (50g×3), the organic phases were combined, washed with saturated brine (100g), dried over anhydrous sodium sulfate, and concentrated by rotary evaporation to obtain the crude pr...
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