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.
Preparing methods of p-aminophenyl-beta-hydroxyethylsulfonyl and p-minophenyl-beta-hydroxyethylsulfonyl sulphonate
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, (2018/06/21)
The invention relates to preparing methods of p-aminophenyl-beta-hydroxyethylsulfonyl and p-minophenyl-beta-hydroxyethylsulfonyl sulphonate. The preparing methods both comprise the steps that p-aminophenyl-beta-hydroxyethylsulfonyl and hydrogen are used as raw materials, modified framework nickel is used as a hydrogen-adding catalyst, a catalytic hydrogenation reaction is conducted in a solvent toobtain reduction liquid, and modified framework nickel and the solvent in the reduction liquid are separated and removed to obtain p-minophenyl-beta-hydroxyethylsulfonyl sulphonate; according to modified framework nickel, nickel is used as a framework, and modified framework nickel is prepared from, by mass, 75-95 parts of Ni, 3-15 parts of Al and 2-10 parts of metal adjuvant; the metal adjuvantcomprises the combination of any one or at least two of Mo, Cu and Cr. The yield can reach 94% or above; preparation of p-minophenyl-beta-hydroxyethylsulfonyl sulphonate is a continuous production technology, the technology is simplified, the production efficiency is high, the quality is stable, the production cost is low, and the economic benefit and social benefit are obvious.
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.
