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Fragmentation sequences - ion mass spectra series n-alkylhalgenides, α, ω-dihaloalkanes, α, ω-dihaloperfluoroalkanes. Effect of terminal halide mass and chain molecular weight 断裂序列。离子质谱系列n-烷基卤化物,α ω-二卤代烷,α ω-二卤全氟烷烃。末端卤化物质量和链分子量的影响
Pub Date : 2022-02-25 DOI: 10.17677/fn20714807.2022.01.03
Nikolay D. Kagramanov
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引用次数: 1
Fluorinated ethers. Communication 3. Preparation of fluorinated ethers by addition of alcohols to epoxides, interaction of fluoroolefins and alcohols with formaldehyde, transesterification, electrochemical fluorination and a number of other methods. 氟醚。沟通3。在环氧化物中加入醇制备氟化醚、氟烯烃和醇与甲醛的相互作用、酯交换、电化学氟化和许多其他方法。
Pub Date : 2022-02-25 DOI: 10.17677/fn20714807.2022.01.01
V. Kornilov
The following methods of obtaining fluorinated ethers are described in the final part of the review: the addition of alcohols to epoxides, the interaction of fluorinated olefins and alcohols with formaldehyde, transetherification, and electrochemical fluorination. In addition, a brief description of methods for obtaining fluorinated ethers that are not included in the separate chapters is given, namely: free radical addition of fluorine-containing alkenes to ethers, fluorination with elemental fluorine and higher fluorides of metals of variable valence, reactions of alcohols with ketones and carboxylic acids, reactions of perfluorinated nitrosoalkanes with alcohols and interaction of alcohols with 2,4,6-tris-(2,2,2-trifluoroethoxy)-[1,3,5]triazine (TriTFET).
本文最后介绍了几种制备氟醚的方法:环氧化物加成醇法、氟化烯烃和氟化醇与甲醛的相互作用法、醚化法和电化学氟化法。此外,还简要介绍了未包括在单独各章中的氟化醚的获取方法,即:含氟烯烃与醚的自由基加成、变价金属与单质氟和高氟化物的氟化、醇与酮和羧酸的反应、全氟亚硝基烷烃与醇的反应以及醇与2,4,6-三-(2,2,2-三氟乙氧基)-[1,3,5]三嗪(TriTFET)的相互作用。
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引用次数: 0
C2-Alkylation in a three-component reaction of fluorocarbonyl compounds, pyrrole derivatives and malononitrile in competition with C2-oxyalkylation 氟羰基化合物、吡咯衍生物和丙二腈三组分反应中的c2 -烷基化与c2 -氧烷基化的竞争
Pub Date : 2022-02-25 DOI: 10.17677/fn20714807.2022.01.02
N. Chkanikov
The C2-alkylation of pyrrole derivatives with 2-(2,2,2-trifluoroethylidene) malononitrile 1, formed in situ from ethyl hemiacetal trifluoroacetaldehyde 2 and malononitrile in the presence of a base, has been carried out. As a result of this three-component reaction, nitriles were obtained derivatives of 4,5,6,7-tetrahydroindole and pyrrole 4a, b, c. A competing reaction is C2-oxyalkylation of the pyrrole ring with hemiacetal 2. It has been shown that the side reaction can be completely suppressed by lowering the reaction temperature to -30∞C. When the ethyl ester of trifluoropyruvic acid 3 reacts with pyrrole derivatives in the presence of malononitrile, the main reaction is the C2-oxyalkylation of the pyrrole ring, rather than its C2-alkylation formed in situ by alkene 10. Nitriles 6 9 were obtained in high yields from pyrrole derivatives and alkene 10. The structure of the compounds was confirmed by 1H, 13C, 19F NMR spectroscopy, mass spectrometry and high-resolution mass spectrometry.
以半缩乙基三氟乙醛2和丙二腈为原料,在碱的存在下原位生成了吡咯衍生物与2-(2,2,2-三氟乙基)丙二腈1的c2 -烷基化反应。通过这种三组分反应,得到了4,5,6,7-四氢吲哚和吡咯4a, b, c的衍生物。与之竞争的反应是吡咯环与半缩醛2的c2 -氧烷基化反应。结果表明,将反应温度降低至-30∞C,副反应完全被抑制。三氟丙酮酸3乙酯在丙二腈存在下与吡咯衍生物反应时,主要反应是吡咯环的c2 -氧烷基化,而不是烯烃10在原位形成的c2 -烷基化。以吡咯衍生物和烯烃10为原料,高收率地得到了腈6 9。化合物的结构通过1H、13C、19F核磁共振谱、质谱和高分辨率质谱证实。
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引用次数: 0
DECARBOXYLATION OF 2,3,3,3-TETRAFLUORO-2-IODOPROPIONIC ACID, ITS POTASSIUM SALT AND TRIMETHYLSILYL ESTER 2,3,3,3-四氟-2-碘丙酸及其钾盐和三甲基硅基酯的脱羧
Pub Date : 2022-02-25 DOI: 10.17677/fn20714807.2022.01.04
S. Igumnov
The preparation of 1,1,1,2-tetrafluoro2-iodoethane by various methods has been studied, it has been shown that the best method is a method in which a solution of acid in dimethylformamide is gradually added to dimethylformamide preheated to 140°C, the mechanism of this reaction with the formation of CF3CFI – anion is proposed.
对制备1,1,1,2-四氟-碘乙烷的各种方法进行了研究,结果表明,将二甲基甲酰胺中的酸溶液逐渐加入到预热至140℃的二甲基甲酰胺中,是制备1,1,1,2-四氟-碘乙烷的最佳方法,并提出了该反应生成CF3CFI -阴离子的机理。
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引用次数: 0
α-Fluoroalkylamines, their properties and application as sources of nucleophilic fluoride ion α-氟烷基胺的性质及其作为亲核氟离子来源的应用
Pub Date : 2021-12-23 DOI: 10.17677/fn20714807.2021.06.02
V. Boyko
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引用次数: 0
Synthesis of fluoride NaYF4/Yb/Tm, NaYF4/Yb/Er micro- and nanocrystals and their characterization by uv optical microscopy method 氟化物NaYF4/Yb/Tm、NaYF4/Yb/Er微纳米晶的合成及紫外光学显微镜表征
Pub Date : 2021-12-23 DOI: 10.17677/fn20714807.2021.06.04
S. Molchanova
Fluoride NaYF4/Yb/Tm and NaYF4/Yb/Er microand nanocrystals, which are in the cubic (alpha-) and hexagonal (beta-) phase, have been synthesized. The sizes, crystal structure and shape of crystals (phosphors) are characterized by methods of scanning electron microscopy and Xray diffraction, as well as by high-resolution UV optical microscopy and confocal microscopy. The photoluminescence (PL) of individual phosphors and their agglomerates in upconversion was studied using IR laser pumping light with wavelength of 980 nm. It was shown that using UV microscopy with wavelength of 365 nm and confocal microscopy with wavelength of 405 nm, it is possible to determine the size and shape of particles with diameter of 300 nm. These methods occupy an intermediate position between optical microscopy (within visible range) and electron microscopy in terms of spatial resolution and are useful while analyzing of nanophosphors with organic cladding based on oleic acid.
合成了立方(α -)相和六方(β -)相的氟化物NaYF4/Yb/Tm和NaYF4/Yb/Er微纳米晶体。通过扫描电子显微镜和x射线衍射以及高分辨率紫外光学显微镜和共聚焦显微镜对晶体(荧光粉)的尺寸、晶体结构和形状进行了表征。利用波长为980 nm的红外激光抽运光,研究了单个荧光粉及其团块在上转换过程中的光致发光特性。结果表明,使用波长为365 nm的紫外显微镜和波长为405 nm的共聚焦显微镜,可以确定直径为300 nm的颗粒的大小和形状。这些方法在空间分辨率上介于光学显微镜(可见光范围内)和电子显微镜之间,在分析油酸有机包层纳米荧光粉时非常有用。
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引用次数: 0
Refraction of amorphous copolymers of perfluoro-2,2-dimethyl-1,3-dioxole and perfluoropropylvinyl ether within a telecommunication wavelength ranges near 1300 and 1550 nm 全氟-2,2-二甲基-1,3-二恶唑和全氟丙基乙烯醚的无定形共聚物在1300和1550 nm附近的电信波长范围内的折射
Pub Date : 2021-12-23 DOI: 10.17677/fn20714807.2021.06.03
E. Polunin
Amorphous copolymers of perfluoro-2,2-dimethyl-1,3-dioxole and perfluoropropyl vinyl ether were synthesized by ultrahigh pressure method without using of initiators. By applying spectroscopic refractometry method, authors measured the refraction (refractive index n(l) and material dispersion dn(l)/dl, where l is a wavelength of optical copolymers radiation) within a telecommunication wavelength ranges near l = 1300 and 1550 nm. It is shown that it have low values of n(l) and small material dispersion dn(l)/dl. Synthesized copolymers can be used as a cladding of silica fibers for high-speed optical information transmission systems, as well as a cladding of waveguides made of fluorine-containing electro-optical polymers for high-speed light modulators.
采用超高压法合成了全氟-2,2-二甲基-1,3-二恶唑与全氟丙基乙烯醚的非晶态共聚物。利用光谱折射法测量了l = 1300 nm和1550 nm附近电信波长范围内的折射率(折射率n(l))和材料色散dn(l)/dl,其中l为光学共聚物辐射波长。结果表明,它具有较低的n(l)值和较小的物料分散dn(l)/dl。合成的共聚物可用于高速光信息传输系统的硅纤维包层,也可用于高速光调制器的含氟电光聚合物波导包层。
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引用次数: 0
Synthesis of lithium (perfluoroalkyl)trihydroaluminates Li[RFAlH3] 全氟烷基三氢铝酸锂Li[RFAlH3]的合成
Pub Date : 2021-12-23 DOI: 10.17677/fn20714807.2021.06.01
A. Tyutyunov
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引用次数: 0
Ionic series in mass spectra of trifluoromethyl-substituted heterocycles and cyclopropanes not containing regular fragment groups 不含规则片段基团的三氟甲基取代杂环和环丙烷质谱中的离子系列
Pub Date : 2021-10-24 DOI: 10.17677/fn20714807.2021.05.03
Nikolay D. Kagramanov
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引用次数: 0
Fluorinated ethers. Communication 2. Preparation of fluorinated ethers by the reaction of fluorinated alcohols with diazomethane, addition of polyfluoroalkyl iodides to alkenes, intermolecular dehydration, addition of perfluoroalkyl hypohalogenites to alkenes and pyrolysis of derivatives of perfluor 氟醚。沟通2。用氟化醇与重氮甲烷反应制备氟醚、在烯烃上加成多氟烷基碘化物、分子间脱水、在烯烃上加成全氟烷基次卤化物以及全氟衍生物的热解
Pub Date : 2021-10-24 DOI: 10.17677/fn20714807.2021.05.04
V. Kornilov
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引用次数: 0
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