Green synthesis method of 4-pyridine sulfonic acid
A technology for green synthesis and pyridine sulfonic acid, applied in the field of green synthesis of 4-pyridine sulfonic acid, can solve the problems of difficult preparation, low conversion rate and yield of raw materials, pungent taste and the like, and achieves easy availability of raw materials and simple raw materials. , the effect of reducing the difficulty of reaction
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Embodiment 1
[0029] Step (1), in the four-necked flask, add 100g 4-chloropyridine, 100g hydrogen peroxide (mass fraction is 27.5%), 100g purified water, 3g TS-1 titanium silicon molecular sieve (Dalian Multiphase Catalyst Co., Ltd.), mechanical Stir, condense and reflux, then heat to 80 ° C, use liquid chromatography to monitor the reaction process, react for 2 hours, after the reaction is completed, filter out the TS-1 titanium silicon molecular sieve, and use liquid alkali (mass fraction is 20%) to adjust the filtrate. The pH was to neutral, the conversion of 4-chloropyridine was 100%, and the yield of 4-chloropyridine nitrogen oxide was 98%.
[0030] Step (2), adding the pH-neutral filtrate obtained in step (1) into a 1-liter autoclave, adding 260 g of sodium sulfite heptahydrate, stirring and dissolving, warming up to 120 ° C, and the reaction pressure is 0.5 MPa, using liquid chromatography. The reaction progress was monitored, and the reaction was carried out for 14 hours. At this ti...
Embodiment 2
[0033] Step (1), in the four-necked flask, add 100g 4-chloropyridine, 100g hydrogen peroxide (mass fraction is 27.5%), 100g purified water, 3g TS-1 titanium silicon molecular sieve (Dalian Multiphase Catalyst Co., Ltd.), mechanical Stir, condense and reflux, then heat to 80 ° C, use liquid chromatography to monitor the reaction process, react for 2 hours, after the reaction is completed, filter out the TS-1 titanium silicon molecular sieve, and use liquid alkali (mass fraction is 20%) to adjust the filtrate. pH to neutral, the conversion of 4-chloropyridine was 100%, and the yield of 4-chloropyridine nitrogen oxide was 98%.
[0034] Step (2), adding the pH-neutral filtrate obtained in step (1) into a 1-liter autoclave, adding 260 g of sodium sulfite heptahydrate, stirring and dissolving, warming up to 120° C., the reaction pressure being 0.5 MPa, and monitoring by liquid chromatography. The reaction progressed for 14 hours. At this time, the conversion rate of 4-chloropyridine...
Embodiment 3
[0037] Step (1), in the four-necked flask, add 100g 4-chloropyridine, 100g hydrogen peroxide (mass fraction is 27.5%), 100g purified water, 3g TS-1 titanium silicon molecular sieve (Dalian Multiphase Catalyst Co., Ltd.), mechanical Stir, condense and reflux, then heat to 80 ° C, use liquid chromatography to monitor the reaction process, react for 2 hours, after the reaction is completed, filter out the TS-1 titanium silicon molecular sieve, and use liquid alkali (mass fraction is 20%) to adjust the filtrate. pH to neutral, the conversion of 4-chloropyridine was 100%, and the yield of 4-chloropyridine nitrogen oxide was 98%.
[0038] Step (2), adding the pH neutral filtrate into a 1-liter autoclave, adding 275g of sodium sulfite heptahydrate simultaneously, stirring and dissolving, warming up to 125 ° C, the reaction pressure is 0.5MPa, using liquid chromatography to monitor the reaction progress, reaction 12 Within hours, the conversion of 4-chloropyridine nitroxide was 100%, ...
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