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带功能基的全氟(烷基乙烯基)醚的研究 Ⅱ.全氟(5-甲基-4,7-二氧杂-Δ~8-壬酸)甲酯的合成
Studies on Perfluoroalkyl Vinyl Ethers with Functional Groups——II. Synthesis of methyl perfluoro-(5-methyl-4, 7-dioxa-Δ~7-nonanoate)
【摘要】 <正> 本文报道全氟4-甲基-3,6-二氧杂-Δ~7-辛基亚磺酸钠(1)的制备及其反应,并应用于合成标题化合物。全氟4-甲基-3,6-二氧杂-Δ~7-辛基磺酰氟(2)在亚硫酸钠水溶液中回流加热即可转变成1,但反应较慢且不完全,如用等体积水和乙腈的混合溶剂,则反应可在6—8小时内完成。
【Abstract】 A useful fluoromonomer methyl perfluoro-5-methyl-4, 7-dioxa-△7-nonanoate wassynthesized by the following route. In H2O-CH3CN perfluoro-3, 6-dioxa-△7-octylsulfonyl fluoride was reduced with Na2SO3 to give sodium perfluoro-4-methyl-3,6-dioxa-△7-octyl sulfinate, which was converted into 8-iodo-perfluoro-5-methyl-3, 6-dioxaoctene-1 by reaction with iodine and KI in water. The carboxylatodeoidination of8-iodo-perfluoro-5-methyl-3, 6-dioxaoctene-l with Zn powder and CO2 in DMFfollowed by esterification of the acid with methanol and sulfuric acid give the titleproduct. It was demonstrated, that FO2SCF2CF2OCF2CF2I and FO2SCF2CF20(CF2)4I canbe carboxylatodeiodinated under the same conditions as 8-iodo-perfluoro-5-methyl-3,6-dioxaoctene-1.
- 【文献出处】 化学学报 ,Acta Chimica Sinica , 编辑部邮箱 ,1989年07期
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