1072-53-3Relevant articles and documents
Ham
, p. 864 (1960)
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Kaiser et al.
, p. 602 (1963)
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Baker,Field
, p. 86,87 (1932)
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Lipkin,Layloff
, p. 450,451 (1970)
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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 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.