- Synthesis method of heptafluoroisobutyronitrile
-
The invention discloses a synthesis method of heptafluoroisobutyronitrile, which comprises the following steps: (1) reacting hexafluoropropylene with carbon dioxide under the catalysis of fluoride salt to obtain heptafluoroisobutyrate; (2) acidifying the obtained heptafluoroisobutyric acid, and then carrying out esterification reaction with alcohol to obtain heptafluoroisobutyrate; and (3) reacting the obtained heptafluoroisobutyrate with ammonia, and dehydrating to obtain heptafluoroisobutyronitrile. The synthesis method has the advantages of easily available raw materials, mild reaction conditions, high reaction conversion rate and yield, easy separation and purification, simple and safe process operation, short synthesis route and low cost.
- -
-
Paragraph 0085; 0089-0091; 0096; 0100-0102
(2021/03/05)
-
- A novel and efficient synthetic route to perfluoroisobutyronitrile from perfluoroisobutyryl acid
-
A novel synthetic route to perfluoroisobutyronitrile from perfluoroisobutyryl acid which has mild conditions and low toxicity is described. This study introduces detailed synthetic protocols and characterization including GC-MS, 13C NMR and 19F NMR spectroscopy of perfluoroisobutyryl acid, perfluoroisobutyryl chloride, perfluoroisobutyl amide and perfluoroisobutyronitrile. Besides, this route is superior to the established patent and shows potential application in high voltage electrical equipment.
- Wang, Yi,Sun, Mengting,Gao, Zhanyang,Zou, Lilin,Zhong, Lingyu,Peng, Ruichao,Yu, Ping,Luo, Yunbai
-
p. 37159 - 37164
(2018/11/26)
-
- Method for preparing heptafluorobutyl chloride from heptafluoro-2-haloalkane
-
The invention discloses a method for preparing heptafluorobutyl chloride from heptafluoro-2-haloalkane. The reaction is divided into two steps: (1) introducing carbon dioxide into a solution A containing metal M under ultrasonic or high-pressure conditions, dropping heptafluoro-2-haloalkane, reacting at a temperature of 60-75 DEG C, acidifying the reaction solution to a pH value of being less than2 after reaction completion, and separating to remove the aqueous phase to obtain an intermediate heptafluoroisobutyric acid; (2) dropwise adding a halogenating agent into solvent-free heptafluoroisobutyric acid under nitrogen protection, stirring and reacting at a room temperature after dropping completion, raising the temperature to perform reflux reaction, observing and stopping the reaction after any gas is not produced, distilling and collecting the fraction of 50 DEG C or below, thereby obtaining the heptafluorobutyl chloride. The method disclosed by the invention has the advantages ofshort synthetic route, simple process flow and low equipment investment.
- -
-
Paragraph 0029; 0030; 0033
(2018/07/30)
-
- Free-radical selective functionalization of 1,4-naphthoquinones by perfluorodiacyl peroxides
-
Perfluoroalkyl radicals, generated by thermal decomposition of perfluorodiacyl peroxides, react selectively with quinone rings of 1,4-naphthoquinones. In the presence of a non-conjugated alkene such as 1-hexene, perfluoroalkyl radicals add to the double bonds of the olefin forming a radical adduct, which selectively adds to the naphthoquinone ring. Several perfluorodiacyl peroxides have been synthesized and used for the direct and alkene-mediated functionalization of naphthoquinones. Geometrical parameters and electron density topology of all perfluorodiacyl peroxides have been calculated by the density functional formalism and quantum theory of atoms in molecules to attempt a rationalization of the experimental reactivity.
- Sansotera, Maurizio,Gambarotti, Cristian,Famulari, Antonino,Baggioli, Alberto,Soave, Raffaella,Venturini, Francesco,Meille, Stefano V.,Wlassics, Ivan,Navarrini, Walter
-
p. 5298 - 5309
(2014/07/08)
-
- Free radical and isomerisation processes during the electrochemical fluorination of n-butyryl chloride, i-butyryl chloride and pivaloyl chloride in anhydrous hydrogen fluoride
-
Electrochemical perfluorination (ECPF) of the title compounds containing primary, secondary and tertiary carbon atoms was carried out in anhydrous hydrofluoric acid (AHF). Detailed analysis of major and minor products suggest that carbon chain isomerisation involving cyclo-propane intermediate is more prevalent during ECPF of i-butyryl chloride when compared to n-butyryl chloride. Simple statistical probability involving free radical intermediates also support this observation. ECPF involving cyclo-propane intermediate is even more prevalent in pivaloyl chloride containing three methyl substituents. In this case, perfluorinated cyclo-propane intermediates were also observed in the product sample. Distribution of minor perfluorinated and partially fluorinated products also suggest the predominant role of normal free radical pathway involving single-electron transfer.
- Velayutham,Jayaraman,Kulangiappar,Ilayaraja,Babu, Y. Ram,Rao, P. Santhan,Reddy, S. Narayana,Babu, K. Victor,Noel
-
p. 1111 - 1118
(2008/09/16)
-
- α-Branched-perfluorodiacyl peroxides: Preparation and characterization
-
New perfluorodiacyl peroxides substituted at the α position have been synthesized and characterized. This class of peroxides shows good hydrolytic stability.
- Galimberti, Marco,Barchiesi, Emma,Navarrini, Walter
-
p. 587 - 593
(2007/10/03)
-
- EPR studies of anion-radicals formed by reduction of perfluorinated α-triketones with some metals of groups I-III
-
Reaction of α,β-bis-fluorosulfatoketones i-C3F7(CFOSO2F)2C(O)RF, (RF=C2F5, i-C3F7) with AcONa/AcOH afforded perfluoro-α-triketones i-C3/sub
- Shaposhnikova,Sterlin,Solodovnikov,Bubnov,Tumanskii
-
-
- Ozonolysis of perfluoroalkenes and perfluorocycloalkenes
-
Ozonolysis of 1-methoxyperfluorocyclobutene in Freon-113 followed by hydrogenation of the reaction products gave methyl hydrogen perfluorosuccinate. Under similar conditions, perfluorooct-1- and -2-enes and 4-trifluoromethyl-1,1,1,2,3,4,5,5,5-nonafluoropent-2-ene were converted into perfluorinated heptanoic, hexanoic, and isobutyric acids, respectively.
- Odinokov,Akhmetova,Savchenko,Bazunova,Fatykhov,Zapevalov
-
p. 1190 - 1191
(2007/10/03)
-
- On reactions of carbon disulphide induced by 'naked' fluoride part 2: Reactions with 2-H-heptafluoropropane, hexafluoropropene, and bis (2,2,2-trifluoroethyl) amine
-
The reaction of CS2 and tetramethylammonium fluoride (TMAF) with 2-H-heptafluoropropane (R227) leads to 2,4-bis(hexafluoroisopropylidene)-1,3-dithietane as well as to the tetramethylammonium salt of heptafluorodithioisobutyric acid. The latter anion resulted also from the reaction of CS2 and CsF with hexafluoropropene (HFP), whereas CS2, TMAF and HFP reacted to compounds derived from HFP dimerization. N,N-bis (2,2,2-trifluoroethyl) dithiocarbamic acid anion was obtained from bis (trifluoroethyl) amine reacted with CS2 and TMAF.
- Ruediger, Stephan,Seppelt, Konrad
-
-
- Tandem Nucleophilic Additions of Aryloxides
-
Hydroquinone disodium salt added sequentially to tetrafluoroethylene and carbon dioxide to yield a symmetrical dicarboxylic acid, which was transformed into the corresponding dimethyl ester, diol, diamide, and diamine.Chlorotrifluoroethylene in analogous reactions gave the corresponding diester and diol in excellent yield.When this kind of transformation was attempted on phloroglucinol, the Kolbe-Schmitt carboxylation reaction intervened.Despite serious competition from addition/elimination processes under typical reaction conditions, the tandem addition of phenoxide ion to hexafluoropropene and carbon dioxide was carried out successfully at lower temperatures and higher carbon dioxide pressures.
- Arnold-Stanton, Regina,Lemal, David M.
-
p. 151 - 157
(2007/10/02)
-
- UTRASOUND-PROMOTED DIRECT CARBOXYLATION OF PERFLUOROALKYL IODIDES
-
Perfluoroalkyl iodides were directly carboxylated with Zn and CO2 under utrasonic irradiation affording the corresponding perfluoroalkanoic acids.
- Ishikawa, Nobuo,Takahashi, Mitsuru,Sato, Takehiko,Kitazume, Tomoya
-
p. 585 - 588
(2007/10/02)
-