- Preparation method of dye intermediate 3-(beta-hydroxyethyl sulfonyl) aniline
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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.
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- Preparation method of meta-ester and meta-ester (by machine translation)
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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)
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- Preparation method of dye intermediate 3-(beta-hydroxyethyl sulfonyl)-nitrobenzene
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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.
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- Preparation method of M-nitro - β β-hydroxyethyl sulfone (by machine translation)
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The invention discloses a method for preparing M-nitro - β β-hydroxyethyl sulfone, belongs to the technical field of dye chemical intermediate manufacturing, and comprises the following steps: (1) adding an aqueous hydrazine hydrate solution, slowly or repeatedly adding m-nitrobenzenesulfonyl chloride; 40~70 °C) dropwise adding ethylene oxide, controlling 50~70 °C the temperature 0.5~1.5, and 2 using pH7.0~7.6 dilute sulfuric acid to maintain pH5.0~7.0, filtering, and obtaining m-hydroxyethyl sulfone. (Z - β β-hydroxyethyl sulfone). Compared with a traditional process for improving the high-salinity wastewater and the nunitz ? waste residue, the process is cleaner, environment-friendly; the process is simple, the required equipment is few, and the investment of equipment is greatly reduced; and the equipment investment can be greatly reduced. 20% 5 tonnes 98.5% 70 kg (by machine translation)
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Paragraph 0031; 0037-0039; 0040; 0042; 0043; 0045; 0046
(2019/09/14)
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- Pteridinone derivatives as PI3-kinases inhibitors
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New compounds of formula 1 are provided which by virtue of their pharmaceutical activity as PI3-kinase modulators may be used in the therapeutic field for the treatment of inflammatory or allergic diseases. Examples of these include inflammatory and allergic respiratory complaints, inflammatory diseases of the gastro-intestinal tract and motor apparatus, inflammatory and allergic skin diseases, inflammatory eye diseases, diseases of the nasal mucosa, inflammatory or allergic conditions involving autoimmune reactions or inflammations of the kidney.
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Page/Page column 17
(2008/12/07)
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- Process for producing [2-(arylsulfonyl) ethenyl] benzene derivatives
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The present invention provides a safer and more efficient process for producing [2-(arylsulfonyl)ethenyl]benzene derivatives of the formula (3): wherein R1, R2, R3 and R4 are the same or different and each independently represent a hydrogen, fluorine, or chlorine atom, a lower alkyl group, or the like, and two adjacent R3 and R4 may bond each other at their terminals to form a ring, which the process is characterized in that a 2-(arylsulfonyl)ethanol of formula (1): wherein R1 and R2 are as defined above, and an acid anhydride are reacted in the presence of a base, and the reaction liquid obtained is supplied to a reaction with an aromatic halide of formula (2): wherein X represents a chlorine, bromine, or iodine atom, and R3 and R4 are the same as defined above, in the presence of a palladium catalyst and a base.
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