90 results about "Chlorosulfonyl isocyanate" patented technology

The invention relates to the field of chemical synthesizing, in particular to a preparation method of imidodisulfuryl fluoride lithium salt. The preparation method includes the steps of firstly, allowing chlorosulfonic acid and chlorosulfonyl isocyanate to react in the presence of catalyst to obtain dichlorosulfimide; secondly, allowing dichlorosulfimide and hydrogen fluoride to react in the presence of catalyst to obtain imidodisulfuryl fluoride; thirdly, allowing imidodisulfuryl fluoride to react with compound containing lithium to obtain the imidodisulfuryl fluoride lithium salt. The preparation method has the advantages that the chlorosulfonic acid and chlorosulfonyl isocyanate are used as the raw materials in the first-step reaction, the generation of waste gases such as SO2 and HCl is avoided, and environment protection requirements are satisfied.

The invention relates to the field of chemical synthesizing, in particular to a preparation method of imidodisulfuryl fluoride lithium salt. The preparation method includes the steps of firstly, allowing chlorosulfonic acid and chlorosulfonyl isocyanate to react in the presence of catalyst to obtain dichlorosulfimide; secondly, allowing dichlorosulfimide and hydrogen fluoride to react in the presence of catalyst to obtain imidodisulfuryl fluoride; thirdly, allowing imidodisulfuryl fluoride to react with compound containing lithium to obtain the imidodisulfuryl fluoride lithium salt. The preparation method has the advantages that the chlorosulfonic acid and chlorosulfonyl isocyanate are used as the raw materials in the first-step reaction, the generation of waste gases such as SO2 and HCl is avoided, and environment protection requirements are satisfied.

The invention relates to the field of chemical synthesis, in particular to a preparation method of potassium bis(fluorosulfonyl)imide. The preparation method comprises the following steps: 1) carrying out a reaction between chlorosulfonic acid and chlorosulfonyl isocyanate to obtain bis(chlorosulfonyl)imide in the presence of a catalyst; 2) carrying out a reaction between the bis(chlorosulfonyl)imide and hydrogen fluoride in the presence of a catalyst to obtain bis(fluorosulfonyl)imide; 3) carrying out a reaction between the bis(fluorosulfonyl)imide and an alkaline potassium compound to obtain the potassium bis(fluorosulfonyl)imide. According to the preparation method provided by the invention, the chlorosulfonic acid and the chlorosulfonyl isocyanate can be used as raw materials in the first step, so that generation of waste gases such as SO2, HCl and the like is avoided, and thus a requirement on environment friendliness can be met better.

The invention provides a synthesis method of high-purity chlorosulfonyl isocyanate. The synthesis method includes the steps that (A) under the condition of a diluent, sulfur trioxide and cyanogen chloride are subjected to sulfonation reaction to obtain a reaction solution; (B) the reaction solution is subjected to thermal decomposition reaction to obtain a reaction solution after thermal decomposition; (C) the reaction solution after thermal decomposition is subjected to positive pressure continuous distillation to obtain the high-purity chlorosulfonyl isocyanate and a distillate before distillation; and the diluent is selected from the chlorosulfonyl isocyanate or the distillate before distillation. According to the synthesis method of the high-purity chlorosulfonyl isocyanate, the totalyield of the process is increased; the distillate before distillation is used as a reaction solvent, use of a high boiling point solvent is avoided, in the pyrolysis process, the cyanogen chloride andthe sulfur trioxide are partially recovered, thus the utilization rate of raw materials is increased, and the production cost is lowered; and meanwhile, the rectification process is conducted throughthe mode of positive pressure distillation and continuous feeding, the yield of products is greatly increased, the distillation time is shortened, energy consumption and labor costs are lowered, andthe synthesis method of the high-purity chlorosulfonyl isocyanate is suitable for industrial mass production.

The invention relates to a method for producing chlorosulfonyl isocyanate by taking cyanogen chloride and sulfur trioxide as raw materials, belonging to the methods for producing chlorosulfonyl isocyanate. The method comprises the following steps: feeding the raw materials into a tubular reactor at a theoretical molar ratio, enabling the raw materials to react continuously in the tubular reactor, feeding the by-products of reaction into a tubular thermal decomposition reactor of by-products, continuously converting the by-products of reaction to the desired product, separating the crude product, and purifying to obtain the high-purity chlorosulfonyl isocyanate. The method provided by the invention can realize the production of the chlorosulfonyl isocyanate through continuous reaction in the tubular reactor, and the method has the advantages of low investment in devices, high production efficiency and strong production capacity. The advanced production process is adopted to produce the chlorosulfonyl isocyanate, a few by-products are generated during reaction in the tubular reactor, and the by-products can be completely converted into the target product through thermal decomposition reaction. No by-product is sent out of the bound in addition to the impurities involved into the raw materials in the production process, the utilization rate of the raw materials is high, the product has high quality, the production process is stable, and the method is easy to operate and has large operating flexibility.

The invention discloses original quality cefuroxime acid and a drug preparation thereof. A preparation method of original quality cefuroxime acid comprises the following steps: (1), adding SMIA, dibenzothiazyl disulfide, phenylamine, dichloromethane, acetonitrile and triethylamine into a reaction bottle, stirring and increasing the temperature, dropwise adding triethyl phosphate, carrying out thermal reaction, cooling for crystallization, carrying out suction filtration, and drying to obtain an intermediate 1; (2), after hydrolyzing, crystallizing 7-ACA, filtering, and drying to obtain an intermediate 2; (3), in a tetrahydrofuran solvent, enabling the intermediate 1 and the intermediate 2 to be subjected to N-acylation reaction, after reaction, dropwise adding chlorosulfonyl isocyanate, and hydrolyzing to obtain cefuroxime acid reaction liquid; (4), purifying the cefuroxime acid reaction liquid to obtain cefuroxime acid products. The preparation method can effectively reduce the content of isomers and solve the residue problem of an accelerator M, is easy to operate, reliable in quality, and suitable for large-scale industrial production.

A process for preparing Oxcarbazepine IIIcomprising:a) reacting oximinostilbene IV with chlorosulfonyl isocyanate in an inert organic solvent and isolating compound Vb) hydrolyzing compound V to form crude Oxcarbazepine IIIc) purifying oxcarbazepine.

The invention relates to a method for synthesizing cefuroxime sodium, which comprises the following steps: 1, performing the N- acylation reaction of 3-deacetyl-7aminocephalosporanic acid and methoxyaminofuranyl ammonium salt which serve as raw materials and adjusting the pH value with hydrochloric acid to less than 7 in a mixed solvent phase to precipitate crystals to obtain 3-deoxyformyl cefuroxime acid; 2, performing the addition reaction of the 3-deoxyformyl cefuroxime acid and chlorosulfonyl isocyanate serving as a strong ammonia formylating agent in an organic solvent to obtain chlorosulfonyl cefuroxime acid, dehydrating the chlorosulfonyl cefuroxime acid to obtain the cefuroxime acid, decarburizing and concentrating the cefuroxime acid, crystallizing the cefuroxime acid in a solvent phase, and drying the crystals under vacuum to obtain a solid product of cefuroxime acid; and 3, dissolving the cefuroxime acid in alkaline solution, decarburizing the resulting product, crystallizing the resulting product in a mixed solvent phase, filtering crystals, and drying the crystals under vacuum to obtain the cefuroxime sodium.