377-38-8Relevant articles and documents
HIGHLY FLUORINATED HETEROCYCLES. PART XVI. POLYFLUORINATED DERIVATIVES OF 1-METHYLPYRROLIDINE, 1-METHYLPYRROL-3-INE AND 1-METHYLPYRROLE
Coe, Paul L.,Holton, Andrew G.,Sleigh, John H.,Smith, Peter,Tatlow, John Colin
, p. 287 - 298 (1983)
Fluorination of 1-methylpyrrole with cobalt(III) fluoride gave six major products, 1-fluoromethyl- and 1-difluoromethyl- -octa-,-3H-hepta-, and -3H,4H-hexa-fluoropyrrolidine.Similar fluorination of 1-methyl-pyrrolidine gave better total recoveries of the same six products, together with 1-trifluoromethyloctafluoropyrrolidine, and 1-fluoromethyl- and 1-difluoromethyl- -2H-heptafluoropyrrolidine. 1-Fluoromethyl- and 1-difluoromethyl- -3H-heptafluoropyrrolidine each gave the corresponding polyfluoropyrrol-3-ine on dehydrofluorination with potassium hydroxide, but the 1-difluoromethyl-2H-heptafluoride could not be dehydrofluorinated. 1-Methyl- and 1-fluoromethyl- -3H,4H-hexafluoropyrrolidine similarly gave the corresponding 3H-3-ine, but no pyrrole.Reaction of 1-methyl-3H,4H-hexafluoropyrrolidine with 'old' aluminium chloride gave a little 1-methyl-2,5-dichlorodifluoropyrrole, the only fluoropyrrole we have obtained so far.Freshly sublimed AlCl3 afforded 1-methyltetrachloropyrrole (obtained also from 1-methylpyrrole and sulphuryl chloride) : fluorination of this with KCo(III)F4 gave 1-methyl- and 1-fluoromethyl- -3,4-dichloro-tetrafluoropyrrol-3-ine.
Production process of fluorine-containing carboxylic acid
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Paragraph 0029-0031; 0052, (2020/07/13)
The invention discloses a production process of fluorine-containing carboxylic acid. The method comprises the following steps: by taking fluorine-containing olefin as a raw material, carrying out an oxidation reaction to obtain fluorine-containing carboxylate, reacting the fluorine-containing carboxylate with an acylating chlorination reagent to obtain a corresponding mixture of fluorine-containing acyl chloride and fluorine-containing acid anhydride, and hydrolyzing and drying the mixture of fluorine-containing acyl chloride and fluorine-containing acid anhydride to prepare the high-purity fluorine-containing carboxylic acid. The method provided by the invention is suitable for post-treatment of fluorine-containing carboxylic acid prepared by a fluorine-containing olefin (monoolefine, diene, cycloolefin and the like) oxidation method, replaces the traditional strong acid acidification and ether continuous extraction process, and is simpler, more convenient and more applicable; the purity of the fluorine-containing carboxylic acid prepared by the method can reach 98% or above.
Method for preparing fluorine-containing binary acyl fluoride from fluorine-containing cycloolefin
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Paragraph 0054, (2020/07/13)
The invention discloses a method for preparing fluorine-containing diacyl fluoride from fluorine-containing cycloolefin, which comprises the following steps: A) oxidizing fluorine-containing cycloolefin serving as a raw material by using an oxidant under the action of a solvent and a catalyst to generate corresponding fluorine-containing dicarboxylic acid; B) under the action of a solvent and a catalyst, subjecting the fluorine-containing dicarboxylic acid prepared in the step A and a fluorination reaction reagent to a fluorination reaction to obtain fluorine-containing diacyl fluoride. The method comprises the following steps: carrying out oxidation reaction on the fluorine-containing cycloolefin to generate corresponding fluorine-containing dicarboxylic acid; directly fluorinating the fluorine-containing dicarboxylic acid into the corresponding fluorine-containing binary acyl fluoride under the action of an organic solvent and a Lewis acid catalyst. The organic solvent and the specific catalyst are adopted, and other conditions are matched, so that the generation of the corresponding acyl fluoride with high efficiency and high yield from the fluorine-containing cycloolefin can beeffectively promoted.
