13257-95-9Relevant articles and documents
Preparation method of dye intermediate 3-(beta-hydroxyethyl sulfonyl) aniline
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, (2020/04/17)
The invention discloses a preparation method of dye intermediate 3-(beta-hydroxyethyl sulfonyl) aniline. The preparation method comprises the following steps: carrying out chlorosulfonation reaction on nitrobenzene and chlorosulfonic acid to obtain m-nitrobenzenesulfonyl chloride; reducing m-nitrobenzenesulfonyl chloride by using sodium pyrosulfite, and regulating the pH value of a reaction solution to 7.4-7.7 in the reaction process; adding sodium chloride after the reaction is finished, and salting out to obtain a reduction product; wherein the molar ratio of sodium pyrosulfite to m-nitrobenzenesulfonyl chloride to sodium chloride is (0.68-0.685): 1: (0.54-0.58); adding ethylene oxide into the reduction product, controlling the PH value to be 7-7.5, and reacting to obtain a condensationproduct; adopting stannous chloride and a Pd/C catalyst for reducing the condensation product to obtain 3-(beta-hydroxyethyl sulfonyl) aniline, wherein the molar ratio of the condensation product to the Pd/C catalyst is (0.45-0.46): 1: 0.0012. The preparation method provided by the invention can effectively inhibit the generation of byproducts in each process link, not only can improve the productquality, but also reduce environmental pollutants, and has a green and environment-friendly effect.
Preparation method of meta-ester and meta-ester (by machine translation)
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, (2020/06/16)
The molar ratio of the reduction product, the ethylene oxide and the sodium phosphate is 7.4 - 7.7; the molar ratio of the reduction product, the ethylene oxide and the sodium phosphate ranges from 0.68 - 0.685: (0.54 - 0.58): 7 - 7.5; the molar ratio Pd / C catalyst in each process link is controlled to 1; the product quality is improved; the environmental pollutants are reduced; and the method has the advantages of environmental protection and environmental protection effects and is obtained by esterification reaction and synthesis of the intermediate ester and Pd / C at PH ranges of (0.52 - 0.63): (0.00.12) 0.0012; and the method comprises the following steps of reducing the product, reducing environmental pollutants and 0.45 - 0.46 reducing environmental pollutants by adding sodium chloride and a Pd/C catalyst to the condensation product after the reaction is complete. (by machine translation)
Preparation method of dye intermediate 3-(beta-hydroxyethyl sulfonyl)-nitrobenzene
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, (2020/05/14)
The invention discloses a preparation method of a dye intermediate 3-(beta-hydroxyethyl sulfonyl)-nitrobenzene. The preparation method comprises the following steps: S1, carrying out chlorosulfonationreaction on nitrobenzene and chlorosulfonic acid to obtain m-nitrobenzenesulfonyl chloride; S2, reducing the m-nitrobenzenesulfonyl chloride by using sodium pyrosulfite, and adjusting the pH value ofthe reaction solution to 7.4-7.7 in the reaction process; adding sodium chloride after the reaction is finished, and salting out to obtain a reduction product, wherein the molar ratio of the sodium pyrosulfite to the m-nitrobenzenesulfonyl chloride to the sodium chloride is (0.68-0.685) : 1 : (0.54-0.58); and S3, adding ethylene oxide and sodium phosphate into the reduction product, controlling the pH value to be 7-7.5, and reacting to obtain 3-(beta-hydroxyethyl sulfonyl)-nitrobenzene, wherein the molar ratio of the reduction product to the ethylene oxide to the sodium phosphate is 1: (0.52-0.63): 0.00.12. The preparatio method effectively inhibits the generation of byproducts in each process link, not only improves the product quality, but also reduces environmental pollutants and has agreen and environment-friendly effect.
Flow cell electrosynthesis of phenylhydroxylamines. In situ reaction with arenesulfonyl chlorides. A convenient route to arenesulfinic acids synthesis.
Moinet, C.,Raoult, E.
, p. 214 - 221 (2007/10/02)
First, electrosyntheses of phenylhydroxylamines in a flow cell fitted with porous cathode and two counter-electrodes are described.Good yields are attained when electrolyses are performed in buffered aqueous organic or aqueous media.Reaction between p-toluenesulfonyl chloride and N-(3-chloro-4-methylphenyl)hydroxylamine, at the outlet of the cell, leads to a N-sulfonylated phenylhydroxylamine (N-addition); hydrolysis of this latter occurs in aqueous basic media to give the corresponding nitrosobenzene and sodium p-toluenesulfinate.As a result, some arenesulfinic acids have been directly obtained after reaction of arenesulfonyl chloride with sodium salt of 3-hydroxylaminobenzoate and 3-hydroxylaminobenzenesulfonate in aqueous phosphate buffer (pH 7).Next, an examination of the reaction of p-toluenesulfonyl chloride with phenylhydroxylamine in organic solvent, in the presence of triethylamine or of sodium carbonate, shows the importance of experimental conditions to control N-addition or O-addition.Addition of some arenesulfonyl chlorides to phenylhydroxylamine, in ether or dichloromethane containing sodium carbonate, gives only the N-sulfonylated phenylhydroxylamines.These compounds lead to nitrosobenzene and arenesulfinate anions in aqueous basic media.Aliphatic or aromatic sulfinic acids can be prepared in this way.
