3741-38-6Relevant articles and documents
Synthesis method of ethylene sulfate
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Paragraph 0027-0032, (2021/04/21)
The invention discloses a synthesis method of ethylene sulfate. The synthesis method comprises the following steps: mixing ethylene sulfite, a first organic solvent, an oxidant calcium hypochlorite solid and a catalyst ruthenium trichloride, adding the mixture into a reaction kettle, and cooling the reaction system to -15 DEG C to 10 DEG C; slowly dropwise adding a certain amount of cold water in a violent stirring state, continuously reacting for 6-10h at the temperature of -10 DEG C to -5 DEG C after dropwise adding is finished, carrying out suction filtration, separating filtrate, washing an organic phase twice by using a small amount of ice water, adding a molecular sieve, performing drying to remove water, performing filtering, performing concentrating, and performing recrystallizing and centrifugal drying to obtain an ethylene sulfate finished product. According to the invention, the synthesis yield of ethylene sulfite is improved; because the common oxidant sodium hypochlorite solution is easy to decompose after being stored at normal temperature, the calcium hypochlorite solid is convenient to store and can be used immediately after being prepared, and the catalyst is less in dosage and low in cost in the oxidation process of ethylene sulfate.
Synthesis process of ethylene sulfate
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Paragraph 0019-0020; 0022-0023; 0025-0026; 0028-0029; 0031, (2021/02/20)
The invention discloses a synthesis process of ethylene sulfate. The synthesis process comprises the following steps: dissolving ethylene glycol in an organic solvent, dropwisely adding thionyl chloride, reacting at 5-10 DEG C for 1-1.5 hours while keeping the temperature, adding a sodium carbonate solution to regulate the pH value to 7-8, and standing to stratify to obtain an ethylene sulfite-containing mixed solution; adding a catalyst into the mixed solution containing ethylene sulfite, dropwise adding a 70% tert-butyl hydroperoxide aqueous solution for 0.5-1 hour, reacting at 30-40 DEG C for 1-3 hours after dropwise adding, then adding a sodium sulfite solution, standing for layering, carrying out aqueous phase extraction, combining organic phases, carrying out reduced pressure concentration, and recrystallizing to obtain ethylene sulfate. The mixed solution containing the ethylene sulfite is directly subjected to oxidation reaction, so that the technological process is simplified;70% tert-butyl hydroperoxide aqueous solution and copper chloride are adopted, so that the cost is further reduced; and the obtained ethylene sulfate has high yield and purity.
Process for preparation of ethylene sulphate
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Paragraph 0074-0077; 0081-0084; 0088-0091; 0095-0098, (2020/11/05)
The present invention relates to a process for preparation of ethylene sulfate, the process comprises the following steps: (1) providing a mixture of an oxidizing agent and an organic solvent, whereinthe oxidizing agent comprises calcium hypochlorite; and (2) adding ethylene sulfite to the mixture to form the ethylene sulfate. According to the method for preparing the ethylene sulfate, a water system heterogeneous oxidation reaction mode adopted in the prior art is avoided. According to the method, the reaction is directly carried out in an organic solvent, so that the practical problem thatthe ethylene sulfate is decomposed in water is solved from the source, the moisture residue and the free acid residue in the product are remarkably reduced, the reaction yield of the ethylene sulfateis improved, and the purity of the product is improved.
Synthesis method of ethylene sulfate
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Paragraph 0047-0048; 0050-0051; 0053-0054; 0056-0057, (2020/11/25)
The invention discloses a synthesis method of ethylene sulfate. The synthesis method comprises the following steps: adding ethylene glycol into a reaction kettle, and cooling the kettle to 35 DEG C orbelow; adding thionyl chloride into the reaction kettle; raising the temperature of the kettle to 45-60 DEG C, and continuously keeping the temperature for 1-3 hours; when the kettle temperature is 30 to 60 DEG C, vacuumizing to -0.05 MPa to-0.1 MPa; recovering the kettle pressure to the normal pressure, dropwise adding alkali liquor into the reaction kettle when the kettle temperature is 10-40 DEG C, and adjusting the pH value of the kettle liquid to 7.5-8; separating out a lower-layer solution to obtain a finished product of ethylene sulfite; adding a sodium hypochlorite solution into the reaction kettle; dissolving the ethylene sulfate crude product in an organic solvent, and adding ice water into the solution; adding a dehydrating agent into the ethylene sulfate organic solution; concentrating and crystallizing the obtained ethylene sulfate organic solution, and drying the obtained solid; dissolving the primary crystal substance in the organic solvent again, and filtering to obtain a white filter cake. The synthesis method has the advantages of high product yield and high product purity.
Synthesis of Cyclic Sulfite Diesters and their Evaluation as Sulfur Dioxide (SO2) Donors
Malwal, Satish R.,Pardeshi, Kundansingh A.,Chakrapani, Harinath
, p. 1201 - 1205 (2020/02/04)
Although sulfur dioxide (SO2) finds widespread use in the food industry as its hydrated sulfite form, a number of aspects of SO2 biology remain to be completely understood. Of the tools available for intracellular enhancement of SO2 levels, most suffer from poor cell permeability and a lack of control over SO2 release. We report 1,2-cyclic sulfite diesters as a new class of reliable SO2 donors that dissociate in buffer through nucleophilic displacement to produce SO2 with tunable release profiles. We provide data in support of the suitability of these SO2 donors to enhance intracellular SO2 levels more efficiently than sodium bisulfite, the most commonly used SO2 donor for cellular studies.
Synthetic method of battery-grade ethylene sulfate
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Paragraph 0016; 0017; 0018; 0019; 0020; 0021, (2019/04/14)
The invention relates to a synthetic method of battery-grade ethylene sulfate and belongs to the technical field of lithium battery materials. The synthetic method is characterized by comprising the following steps: mixing glycol with an organic solvent, adding sulfoxide chloride, and adding a deacidification agent; continuing to react at the room temperature, filtering, and distilling, so as to obtain vinyl sulfite; mixing vinyl sulfite with an organic peroxide, and adding an initiator for reaction; and carrying out distillation, suction filtration and recrystallization, so as to obtain battery-grade ethylene sulfate. The synthetic method has the beneficial effects that the conditions are mild, the side reaction is avoided, the craft process is simple, the requirements on equipment and environmental protection are low, the product is easily separated and extracted, the contents of moisture and impurities are low, and the prepared product is high in product.
Profiling the oxidative activation of DMSO-F6 by pulse radiolysis and translational potential for radical C-H trifluoromethylation
Santschi, Nico,Jelier, Benson J.,St?helin, Samuel,Nauser, Thomas
supporting information, p. 9734 - 9742 (2019/12/02)
The oxidative activation of the perfluorinated analogue of dimethyl sulfoxide, DMSO-F6, by hydroxyl radicals efficiently produces trifluoromethyl radicals based on pulse radiolysis, laboratory scale experiments, and comparison of rates of reaction for analogous radical systems. In comparison to commercially available precursors, DMSO-F6 proved to be more stable, easier to handle and overall more convenient than leading F3C-reagents and may therefore be an ideal surrogate to study F3C radicals for time-resolved kinetics studies. In addition, we present an improved protocol for the preparation of this largely unexplored reagent.
Preparation method of cyclic sulfite
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Paragraph 0068-0095, (2019/04/06)
The invention relates to a preparation method of cyclic sulfite. Cyclic sulfite is shown as a general formula (I), wherein R1, R2, R3, R4, R5 and R6 can be identical or different and respectively refer to hydrogen, halogen atom substituted or unsubstituted C1-4 alkyl or halogen atom substituted or unsubstituted C2-4 alkenyl, and n is 0, 1 or 2. The preparation method includes: using diol shown asa general formula (II) (wherein, R1, R2, R3, R4, R5, R6 and n are identical with the above definition) and thionyl halide as raw materials, and allowing the raw materials to sequentially pass two reaction temperature areas for continuous reaction, wherein temperature of the first reaction temperature area is set within a range of 25-45 DEG C, and temperature of the second reaction temperature areais set within a range of 50-100 DEG C. The preparation method is high in industrialization feasibility, safe, environment-friendly, catalyst-free, low in raw material cost and capable of preparing high-purity cyclic sulfite with high yield.
Method for preparing ethylene sulfate
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Paragraph 0019; 0020; 0021, (2019/04/09)
The invention relates to a method for preparing ethylene sulfate. According to the technical scheme, the method comprises the following steps: firstly, taking sulfoxide chloride and ethylene glycol asreactive raw materials to carry out a substitution reaction; secondly, adding a catalyst and a buffer agent into the reaction product, and oxidizing with sodium hypochlorite; and thirdly, centrifuging the reactant in the previous step, re-crystallizing, filtering, refining, and drying, thereby obtaining the finished product. The method disclosed by the invention has the beneficial effects that the method has the characteristics of being readily available in reactive raw materials, low in preparation cost, high in molar yield, high in purity of the prepared product and low in moisture content,the reaction can be rapidly and efficiently carried out by the catalyst adopted in the invention, the oxidation time is reduced, and hydrolysis of the ethylene sulfate is reduced. In addition, the mixed aqueous solution of ammonium di-hydrogen phosphate and borax is adopted as a buffer agent needed by oxidation, the oxidative pH value can be effectively controlled to be 6-7, and stable oxidationis promoted. Moreover, by taking magnesium sulfate as a water removal agent, the moisture of the product is controlled to be 50ppm or less.
Synthetic method for ethylene sulfite derivative
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Paragraph 0023-0026, (2018/06/13)
The invention relates to a synthetic method for an ethylene sulfite derivative, and belongs to the field of fine chemical synthesis. The synthetic method comprises the following steps: with titanate as a catalyst, carrying out ester exchange on dimethyl sulfite and corresponding glycol to synthesize the target compound, wherein the using amount of the catalyst is 0.01% to 2% of total weight of reactants, and the mole ratio of the used glycol to the used dimethyl sulfite is 1 to 1.2; reacting at the temperature of 80 to 150 DEG C, gradually carrying out fractionation to remove generated methylalcohol, and stopping the reaction when the methyl alcohol is not fractionated any longer; and carrying out vacuum distillation on the reaction product, and collecting the target substance. The methodhas the advantages of no corrosion, high raw material conversion rate, high yield and the like.
