97-41-6Relevant articles and documents
Synthesis Method of Cyclopropane or Cyclopentene Derivatives via Fe-catalyzed Cationic Radical Cycloaddition Reaction
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Paragraph 0080-0081; 0101-0102, (2021/11/02)
In this disclosure Fe (III) complex is used as an electron oxidizing agent to oxidize an electron - rich alkene compound to form a radical cation intermediate, and then a cyclopropane compound or 3 5-membered ring compound is synthesized by inducing a cycloaddition reaction with the diazo compound.
Cycloaddition Reactions of Alkene Radical Cations using Iron(III)-Phenanthroline Complex
Cho, Yong Hyun,Kim, Jae Hyung,An, Hyeju,Ahn, Kwang-Hyun,Kang, Eun Joo
supporting information, p. 2183 - 2188 (2020/04/29)
Single electron oxidation of electron-rich alkenes using the iron(III)-phenanthroline complex produced electrophilic alkene radical cations, which promoted efficient radical cation [2+1] cycloaddition reactions with diazo compounds. Subsequent chain propagation afforded tri- and tetra-substituted cyclopropanes. This methodology was also expanded to [3+2] cycloaddition reactions with vinyl diazoesters, validating this sustainable, first-row transition metal iron system for the single electron redox reactions. (Figure presented.).
High-yield ethyl chrysanthemate preparation method
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Paragraph 0037-0080, (2020/12/08)
The invention belongs to the technical field of chemical processes, and specifically relates to a high-yield ethyl chrysanthemate preparation method. The high-yield ethyl chrysanthemate preparation method comprises the following steps: (1) diazotization: a step of adding water, glycine ethyl ester acid salt, glacial acetic acid and dimethyl carbonate as solvents into a diazotization kettle, dropwisely adding a sodium nitrite aqueous solution into the diazotization kettle, and carrying out a reaction so as to a diazo liquid; (2) cyclization: a step of putting 2,5-dimethyl-2,4-hexadiene into a cyclization kettle, and carrying out a reaction with cuprous chloride as a catalyst so as to obtain a cyclized solution; (3) desolventizing: a step of sending the cyclized solution into a high-yield desolventizing tower to remove the solvents so as to obtain a crude ethyl chrysanthemate product; and (4) distillation: a step of putting the crude ethyl chrysanthemate product into a distillation kettle, and carrying out vacuum distillation so as to obtain the high-purity ethyl chrysanthemate. The high-yield ethyl chrysanthemate preparation method provided by the invention has the following beneficial effects: when the dimethyl carbonate is used as a solvent, a diazotization reaction can be carried out more completely, so the loss of raw materials is reduced; and meanwhile, the yield of ethyl chrysanthemate in the subsequent cyclization reaction can be improved.