- A process for the preparation of the fluoro method
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The invention relates to a method of preparing fluoroalcohol of which the structure formula is F3C(CF2)nCH2OH, wherein n is an integer of 2-8. The method includes following steps: (I) mixing fluorocarboxylic acid and isopropyl alcohol and performing a temperature-increasing reflux reaction; (II) when the reaction is finished, distilling the reaction liquid to remove generated water and isopropyl alcohol, and cooling the rest reaction liquid to room temperature; (III) pouring the reaction liquid into distillated water, regulating the pH value to 6.5-7 by an alkali liquid, allowing the reaction liquid to stand to layer the reaction liquid to obtain an organic layer; (IV) removing water from the organic layer to obtain fluorocarboxylic isopropyl ester; (V) adding the fluorocarboxylic isopropyl ester and a solvent into a high-pressure reaction kettle with addition of a hydrogenation catalyst and a co-catalyst, sealing the reaction kettle, increasing the temperature and filling hydrogen to a high pressure for performing a reaction for 20-60 h; (VI) when the reaction is finished, cooling the reaction kettle to room temperature, discharging hydrogen to obtain a reaction mixed liquid; (VII) performing rectification to the reaction mixed liquid to separate the solvent, cooling the rest liquid and pouring the rest liquid into distillated water and regulating the pH value to 6.5-7 by an acid liquid; and (VIII) allowing the mixed liquid to stand to layer the mixed liquid to obtain an organic layer, removing water from the organic layer and distilling the organic layer to obtain the corresponding fluoroalcohol.
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- Homogeneous catalytic hydrogenation of perfluoro methyl esters
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The first example of perfluoroalkyl methyl ester RfC(O)OMe (Rf = C3F7, C5F11) reduction by homogeneous catalytic hydrogenation with the ruthenium catalyst Ru-MACHO is herein reported. The hydrogenation process leads to the corresponding perfluorinated alcohols thus replacing sodium borohydride that has so far represented the state of art in perfluoro ester reduction.
- Lazzari, Dario,Cassani, Maria Cristina,Bertola, Maurizio,Moreno, Francisco Casado,Torrente, Damiano
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p. 15582 - 15584
(2013/09/12)
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- Various synthetic approaches to fluoroalkyl p-nitrophenyl ethers
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Homologous 1H,1H-perfluoroalkyl p-nitrophenyl ethers (alkyl = C2-C8) were synthesized using different methods. The results are discussed in context with contradictory comments of the literature. The fluoroalkoxylation of p-chloronitrobenzene occurs in only one step, but it is limited to small fluoroalkyl groups. The fluoroalkylation of p-nitrophenol via sulphonic acid esters is a better synthetic route. Differences in reactivity and yield between tosylates, mesylates and inflates are found and discussed. The preferred synthesis includes the use of trifluoromethane sulphonic acid esters.
- Preschera, Dietrich,Thiele, Thomas,Ruhmann, Ralf
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p. 145 - 148
(2007/10/03)
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