Sulfonium sulfonate salt photoacid generator synthesized from ledol and synthesis method for sulfonium sulfonate salt photoacid generator
The technology of a photoacid generator and trumpet alcohol, which is applied in the field of sulfonate photoacid generators and their synthesis, can solve the problems such as the inability to reduce the edge roughness, and achieve easy preparation, good transparency, and reduced line The effect of wide roughness
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Embodiment 1
[0040] This embodiment provides a kind of sulfonate salt photoacid generator synthesized by trumpet 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 (13g, 325mmol) was dissolved in water (30g) to form a sodium hydroxide solution; methyl fluorosulfonyl difluoroacetate 1-1 (20g, 104mmol) was added to ice water (50g) , to obtain the reaction solution, and slowly add the prepared sodium hydroxide solution to the above reaction solution under stirring, after the addition, the reaction solution was stirred for 2.5 hours in an ice bath (controlling the temperature below 10 degrees Celsius), and then at room temperature After continuing to stir 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...
Embodiment 2
[0048] This embodiment provides a kind of sulfonate salt photoacid generator synthesized by trumpet 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 nitrogen protection at 0°C, add pyridine (16.6g, 90.2mmol), bis(trichloromethyl)carbonate (9g, 30mmol) into dichloromethane (400g), and slowly add it under stirring Trumpetyl alcohol 2-1 (20g, 90mmol) 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 (16.6g , 90.2mmol) was added to 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 added to methyl tert-butyl ether (250g) for beating to obtain a mixed solution, and the above-mentioned The mixed solution was...
Embodiment 3
[0054] This embodiment provides a kind of sulfonate salt photoacid generator synthesized by trumpet 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, slowly add sodium hydride (3.3g, 138mmol) into a mixture of trumpet alcohol 3-1 (20g, 90mmol) and anhydrous tetrahydrofuran (300g), and stir for 20 minutes; then , Ethyl bromoacetate (15g, 90mmol) was added dropwise to the above mixture, and stirred for 20 minutes; then, stirred at 25°C for 6 hours for reaction, after the reaction was completed, quenched with water at 0°C. Concentrate the quenched mixed solution by rotary evaporation, extract three times with dichloromethane (150g×3), combine the extracts, wash and separate the liquids with saturated brine (150g), dry over anhydrous sodium sulfate, and concentrate by rotary evaporation to obtain Crude product; the crude product was ...
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