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本文用不同方法获得含有磺酰氟基的烯烃.利用格氏反应由ω-碘-3-氧杂全氟烷磺酰氟(1)得到了γ-和ω-全氟烯基醚磺酰氟(2b和2c).1可与乙烯加成制得ICH_2CH_2(CF_2CF_2)_(n+1)-OCF_2CF_SO_2F(3),然后用三乙胺脱碘化氢得到相应的烯烃4.含有氟氯双键的磺酰氟6曾从CFCI_2CFCIOCF_2CF_2SO_2F(5)脱氯得到.5与Swarts试剂反应得不到CF_2CICFClOCF_2CF_2SO_2F,却得到醚键的α氯被氟化的7.β-磺酰氟基全氟乙氧基阴离子与对甲苯磺酸β-氯乙酯反应得到5-氯-4,4,5,5-四氢-3-氧杂四氟戊磺酰氟(12),它亦可由四氟乙磺内酯、氟化钾、乙烯、氯在DG中反应制得.经过氯化、脱氯,得到三氯乙烯基醚乙磺酰氟(14). 合成了含有内部双键的对称全氟和多氟醚二磺酰氟.将CFCIICF_2OCF_2CF_2SO_2F(15)在乙酐、二氯甲烷或乙酸乙酯、二氯甲烷中用锌粉偶合,得到(—CFCICF_2OCF_2CF_2SO_2F)_2(16),再脱氯制得(=CFCF_2OCF_2CF_2SO_2F)_2(17).CCI_3CF_2OCF_2CF_2SO_2F(18)在180～200℃可经铜粉进行脱卤偶合而成(=CCICF_2OCF_2CF_2SO_2F)_2(19)。
In this paper, sulfonyl fluoride-containing olefins were obtained by different methods.G- and ω-perfluoroalkylether sulfonyl fluoride were obtained from ω-iodo-3-oxa-perfluoroalkanesulfonyl fluoride (1) (2b and 2c) .1 can be obtained with the addition of ethylene ICH_2CH_2 (CF_2CF_2) _ (n +1) -OCF_2CF_SO_2F (3), and then dehydroiodination with triethylamine to give the corresponding olefin 4. Containing fluorine double bond Of sulfonyl fluoride 6 was obtained from the dechlorination of CFCI_2CFCIOCF_2CF_2SO_2F (5) .5 The reaction with Swarts reagent failed to obtain CF_2CICFClOCF_2CF_2SO_2F, but the ether of α-chlorine was fluorinated by 7.β-sulfonyl fluoride perfluoroethoxy anion Reaction with β-chloroethyl p-toluenesulfonate gives 5-chloro-4,4,5,5-tetrahydro-3-oxa-tetrafluoropentanesulfonyl fluoride (12) , Potassium fluoride, ethylene, chlorine in the DG obtained by the reaction, after chlorination, dechlorination, trichlorovinyl ether ethanesulfonyl fluoride (14) Synthesis of the internal double bond containing the symmetric perfluoro and polyfluoroether (CFCICF_2OCF_2CF_2SO_2F) 2 (CFCICF_2OCF_2CF_2SO_2F) _2 (16) was obtained by the reaction of CFCIICF_2OCF_2CF_2SO_2F (15) with acetic anhydride, methylene chloride or ethyl acetate and methylene chloride, followed by dechlorination (= CFCF_2OCF_2CF_2SO_2F) _2 (17) .CCI_3CF_2OCF_2C F_2SO_2F (18) can be formed by the dehalogenation of copper powder (= CCICF_2OCF_2CF_2SO_2F) _2 (19) at 180 ~ 200 ℃.