2494-89-5Relevant articles and documents
Para-ester synthesis method and para-ester
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Paragraph 0059-0170, (2020/05/05)
The invention discloses a para-ester synthesis method which comprises the following steps: S1, adding a set amount of chlorosulfonic acid and acetanilide into a sulfonation reaction kettle, adding thionyl chloride, and carrying out a reaction to prepare a sulfonated product, wherein the molar ratio of acetanilide to chlorosulfonic acid to thionyl chloride is (0.45-0.46):1:(0.46-0.47); S2, dilutingthe sulfonated substance and then carrying out suction filtration; S3, adding pyronitrite, adjusting a stable pH value, and carrying out a reduction reaction to obtain a reduction solution; S4, taking sodium phosphate as a buffer agent, adding sulfuric acid and ethylene oxide, and carrying out condensation reaction to obtain a condensation product; S5, carrying out suction filtration on the condensation product; S6, adding sulfuric acid into a product obtained after suction filtration, and carrying out an esterification reaction; and S7, crushing and packaging the product obtained after the esterification reaction to prepare the para-ester. The invention also discloses the para-ester. According to the synthetic method disclosed by the invention, the dosage of chlorosulfonic acid is reduced, thionyl chloride is used for replacing part of chlorosulfonic acid, and the para-ester yield is improved by optimizing the ratio.
Method for preparing p-aminophenyl-beta-hydroxyethyl sulfone sulfate
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Paragraph 0009; 0010; 0011, (2018/04/03)
The invention discloses a method for preparing p-aminophenyl-beta-hydroxyethyl sulfone sulfate. The method comprises the following steps: with p-nitrochlorobenzene and mercaptoethanol as basic raw materials, adding into an N,N-dimethylformamide solvent, sufficiently dissolving and uniformly mixing to obtain p-nitrophenyl-beta-hydroxyethyl sulfide, then adding hydrogen peroxide, separating out an oxidization crystallization material, adding solvent water and a palladium-carbon catalyst into the oxidization crystallization material, reacting, filtering to obtain a hydrogenated product and the solvent water, adding the hydrogenated product into an ice-water mixture, diluting, adding pure sulfuric acid, stirring, heating to 150 DEG C, and performing an esterification reaction for 2-3h under avacuum condition to obtain the p-aminophenyl-beta-hydroxyethyl sulfone sulfate after the reaction. The product prepared by the method provided by the invention is high in purity and yield, the raw material consumption is low, the raw material utilization rate is increased, few byproducts are produced and are easy to separate, produced wastewater is easy to treat, and the environmental protection investment is low.
An environment-friendly to-(β-hydroxyethyl sulphone sulfate) method for the synthesis of aniline
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Paragraph 0024-0025, (2017/06/20)
The invention discloses a synthesis method of environmental-friendly p-(beta-sulfatoethylsulfonyl) aniline. The synthesis method comprises the following steps: (1) in the presence of a chlorination inhibitor, carrying out sulfonation reaction on acetanilide and chlorosulfonic acid, and then carrying out chlorination reaction on the obtained product and thionyl chloride, so that a chlorosulfonation substance is obtained; and (2) sequentially carrying out condensation reaction, sulfonating reaction and hydrolysis reaction on the chlorosulfonation substance obtained in the step (1), so that environmental-friendly p-(beta-sulfatoethylsulfonyl) aniline is obtained. According to the preparation method, by changing a production formula, introducing the chlorination inhibitor, and changing the reaction reactivity of reaction raw materials, p-chloroacetanilide byproducts are greatly reduced, so that an effect that a para-ester product parachloroaniline meets the standard is finally achieved.