4426-51-1Relevant articles and documents
Preparation method of 4-methyl-1,3,2-dioxathiane 2-oxide
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Paragraph 0021; 0024-0033, (2018/05/16)
The invention discloses a preparation method of 4-methyl-1,3,2-dioxathiane 2-oxide. The preparation method comprises the following steps: 1, taking 1,3-butylene glycol and thionyl chloride as raw materials, dropwise adding thionyl chloride to 1,3-butylene glycol for a synthesis reaction, and controlling the reaction system temperature to be 35-45 DEG C, so as to obtain a reaction crude product 10-30 min after the thionyl chloride is dropwise added and when the reaction is finished; 2, performing reduced-pressure rotary evaporation on the reaction crude product for acid removal, controlling thetemperature of reduced-pressure rotary evaporation to be 35-45 DEG C and the time to be 15-30 min, so as to obtain a crude product subjected to acid removal; 3, adding an acylation reagent into the crude product subjected to acid removal for a reaction, after the reaction is finished, adding an alkaline aqueous solution until the pH value is 6-7; 4, performing standing layering, separating the organic phase and the aqueous phase, washing the organic phase to obtain a first crude product, and performing extraction on the aqueous phase to obtain a second crude product; and 5, merging the firstcrude product and the second crude product, performing reduced-pressure rectification, so as to obtain the target product 4-methyl-1,3,2-dioxathiane 2-oxide. The preparation method of the invention has the advantages that the yield, productivity and purity are greatly improved.
Chemo- and Regioselective Functionalization of Polyols through Catalytic C(sp3)-C(sp3) Kumada-Type Coupling of Cyclic Sulfate Esters
Ramírez-Contreras, Rodrigo,Morandi, Bill
supporting information, p. 3718 - 3721 (2016/08/16)
This contribution describes a copper-catalyzed, C(sp3)-C(sp3) cross-coupling reaction of cyclic sulfate esters, a distinct class of electrophilic derivatives of polyols, with alkyl Grignard reagents to afford functionalized alcohol products in good yields. The method is operationally simple and highlights the potential of cyclic sulfate esters as highly reactive substrates in catalytic, chemoselective polyol transformations.
2-Oxo-1,3,2-dioxathianes. I. Preparation of the Alkyl-substituted Derivatives
Virtanen, Terttu,Nikander, Hannu
, p. 113 - 116 (2007/10/02)
2-Oxo-1,3,2-dioxathiane, all methyl- and several other alkyl-substituted 2-oxo-1,3,2-dioxathianes have been synthesized by condensing 1,3-alkanediols and thionyl chloride.The amount of the S==O-axial and S==O-equatorial isomers can be controlled by adding pyridine to the reaction mixture.