1072-53-3Relevant academic research and scientific papers
Kinetic resolutions concentrate the minor enantiomer and aid measurement of high enantiomeric purity
Caron,Tseng,Kazlauskas
, p. 83 - 92 (1994)
Although many methods can measure enantiomeric purity, only a few can measure high enantiomeric purity, >98% ee, because in most methods the signal for the major enantiomer overwhelms the signal for the minor enantiomer. We use a kinetic resolution to concentrate the minor enantiomer into the product and thereby extend the ability of all existing techniques to measure high enantiomeric purity. The original enantiomeric purity is calculated using the enantioselectivity of the kinetic resolution and the extent of conversion. We verified this method with samples of (1S)-menthol using an acetylation with vinyl acetate catalyzed by lipase from Candida rugosa. The enantiomeric purities determined by capillary gas chromatography directly and after kinetic resolution agreed for samples with 90-99.9% ee. Error analysis suggests that the usual accuracies for conversion and enantiomeric ratio are sufficient for accurate determination of enantiomeric purity with this method. In another example, we used a kinetic resolution followed by a simple optical rotation measurement to accurately quantify 98.5% ee for a commercial sample of (S)-(+)-6-methoxy-α-methyl-2-naphthaleneacetic acid (naproxen). Thus, this kinetic resolution method allows simple techniques such as optical rotation to measure high enantiomeric purity.
High yield synthesis of cyclic phosphites, phosphates, sulphites and sulphates of catechol and glycol mediated by hypervalent silicon centres
Kingston,Sudheendra Rao
, p. 4841 - 4844 (1997)
Room temperature reactions of both tris(catecholato)silicate, M2[Si(o-C6H4O2)3] {M=Na, Et3NH} and glycolato silicate, K2[Si2(O2C2H4)5] with PCl3, POCl3, SOCl2 and SO2Cl2 proceed exothermally and afford easy isolation of the corresponding cyclic derivatives of catechol/glycol (1-8) in high yield, exemplifying the merit of hypervalent silicon centres in synthesis. (Et3NH)2[Si(o-C6H4O2)3] afford near quantitative conversions.
Preparation method of cyclic sulfate
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Paragraph 0014; 0019-0020, (2021/01/29)
The invention discloses a preparation method of cyclic sulfate, which is used for preparing cyclic sulfate by a one-step method, and has the beneficial effects that an epoxy compound is used as a rawmaterial to react with sulfamic acid or sulfuric acid in one step under the participation of anhydride to prepare cyclic sulfate, and noble metal catalysis is not needed in the preparation process; corrosive gas production is achieved, the product is high in purity and low in chromaticity (less than 20Hazen), the moisture content is less than or equal to 20ppm, and the acid value is less than or equal to 10ppm, and the influence of moisture and acid value in the electrolyte on the cycle performance and storage stability of the battery is effectively changed.
Preparation method of ethylene sulfate derivative
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Paragraph 0027-0028; 0029-0030; 0031-0032; 0035-0040, (2021/01/25)
The invention belongs to the technical field of organic synthetic chemistry, and particularly relates to a preparation method of an ethylene sulfate derivative, which comprises the following steps: ina mixed solvent composed of an organic solvent and water, in the presence of alkali and quaternary ammonium salt, by using ruthenium trichloride as a catalyst, reacting to obtain the ethylene sulfatederivative. The ethylene sulfite derivative shown in the general formula A and trichloroisocyanuric acid shown in the formula TCCA are subjected to an oxidation reaction to obtain the ethylene sulfate derivative, and the reaction route is as follows: R1 to R4 are independently a hydrogen atom or an alkyl group of C1-3; the ethylene sulfate derivative is synthesized with high efficiency and low cost, and the yield and purity of the product are improved.
Synthesis method of ethylene sulfate
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Paragraph 0031; 0033-0044, (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; 0021-0022; 0024-0025; 0027-0028; 0030-0031, (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.
Preparation method and application of cyclic sulfate compound
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Paragraph 0051-0056, (2020/09/23)
The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method and application of a cyclic sulfate compound. One embodiment of the invention provides a preparation method of a cyclic sulfate compound. The cyclic sulfate compound is prepared from a compound A and sulfur-containing oxide, wherein the structural formula of the compound A is shown in the specification, R is selected from one of H, alkyl, alkenyl, substituted alkyl, aryl and halogen, X is C or S, and Y is-CH2-CH2-or-CH = C-. The compound A and sulfur trioxide are reliable in source, low in price, mild in reaction condition, easy to operate, free of waste water in the reaction process, few in three wastes, good in product quality, suitable for large-scale production, capable of obtaining the high-purity battery-grade ethylene sulfate compound, and relatively high in implementation value and social and economic benefits.
Ethylene sulfate preparation method
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Paragraph 0017-0019, (2020/03/02)
The invention relates to an ethylene sulfate preparation method, which comprises: dissolving ethylene glycol in an aprotic organic solvent, adding an aprotic organic alkali, introducing sulfuryl fluoride, stirring while reacting, filtering after the reaction is completed, and carrying out evaporating concentrating and drying on the filtrate to obtain ethylene sulfate. According to the invention, the ethylene sulfate prepared by the method has extremely high purity of more than 99.9%, low moisture content of less than or equal to 20 ppm and low acid value of less than or equal to 10 ppm, and effectively changes the influence of the moisture and the acid value in an electrolytic solution on the cycle performance and the storage stability of a battery.
METHOD OF OXIDIZING USING CALCIUM HYPOCHLORIDE AND MANUFACTURING FOR SULFONE OR SULFIDE
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Paragraph 0111-0114; 0131, (2020/06/11)
Is a process for preparing a sulphone or sulfate compound using calcium hypochlorite, and, wherein the method comprises introducing, sulfoxide or sulfite compound in an organic solvent and adding calcium hypochlorite in a solid state to an organic solvent in which the compound is introduced to oxidize the compound. (by machine translation)
Method for preparing cyclic sulfate by directly oxidizing hydrogen peroxide
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Paragraph 0045-0047, (2020/11/23)
The method comprises the following steps: dropwise adding hydrogen peroxide into a mixture of cyclic sulfite, an organic solvent and a solid catalyst to carry out catalytic oxidation reaction, filtering out the solid catalyst after the reaction is finished, standing filtrate for layering, taking an organic layer, and performing distilling and concentrating to obtain a cyclic sulfate product. Cheaphydrogen peroxide is used for directly catalyzing and oxidizing cyclic sulfite to prepare cyclic sulfate, so that on one hand, the reaction is mild and easy to control, and the reaction conversion rate is high; on the other hand, no waste salt is generated, the evaporation capacity of water is small, energy consumption is low, generated waste water is little, and the production process is more environmentally friendly; the used solid catalyst contains an active component, an active auxiliary agent and an oxide carrier, and can be recycled, so that the consumption of noble metals is reduced, and the production cost is greatly reduced; the cyclic sulfate prepared by the method is few in impurities, high in purity and wide in market prospect.
