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Process for the preparation of oxysulfides and fluorinated compounds

A technology of fluorinated compounds and oxysulfides, applied in the direction of organic chemistry, etc., can solve problems such as limiting the recycling and reuse of starting materials

Active Publication Date: 2021-01-12
RHODIA OPERATIONS SAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Advantageously, this improved process makes it possible to reduce unfavorable continuous reactions, which makes it possible to achieve high selectivities, e.g. , which significantly limits the recycling of starting materials and greatly simplifies the process downstream

Method used

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  • Process for the preparation of oxysulfides and fluorinated compounds

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0085] Example 1: According to the continuous implementation at SO 2 Preparation of trifluoromethane by sulfination of bromotrifluoromethane in the presence of potassium hydroxide Potassium Methanesulfinate CF 3 SO 2 K

[0086] use figure 1 device indicated.

[0087] 300 g of DMF and 33.6 g (0.6 mol) of potassium hydroxide beads were introduced into a circulation loop (3) equipped with a stirrer (2) and a static mixer (4) and equipped with a reflux condenser (5) at the top ) in the 500ml reactor (1). Heating was carried out to 70° C. and sulfur dioxide gas was introduced through the dip tube ( 6 ) to obtain a concentration of 1% by weight in DMF. This concentration level was confirmed by in situ Raman analysis. When the concentration stabilized, gaseous CF was introduced under the pump suction of the circulation loop (7) via route (8) at a flow rate of 10 g / h 3 Br. Introducing CF 3 During this phase of Br, SO in the reactor 2 The concentration was kept at 1% by ...

example 2

[0089] Example 2 (comparison):

[0090] Repeat what is described in Example 1 for the preparation of CF 3 Br method, but with SO in DMF at 5 bar 2 The concentration was adjusted to 10% by weight to carry out the reaction. After analysis of the final crude reaction product, relative to the introduced CF 3 Br, CF 3 SO 2 The yield of K was 33%.

example 3

[0091] Example 3: According to the continuous implementation in SO 2 Preparation of trifluoromethane by sulfinating bromotrifluoromethane in the presence of sodium formate Sodium sulfinate CF 3 SO 2 Na

[0092] use figure 1 device indicated.

[0093] 300 g of DMF and 15 g (0.22 mol) of sodium formate powder were introduced into a 500 ml reaction equipped with a stirrer (2) and a circulation loop (3) equipped with a static mixer (4) and equipped with a reflux condenser (5) at the top device (1). Heating was carried out to 70° C. and sulfur dioxide gas was introduced through the dip tube ( 6 ) to obtain a concentration of 1% by weight in DMF. This concentration level was confirmed by in situ Raman analysis. When the concentration stabilized, gaseous CF was introduced under the pump suction of the circulation loop (7) via route (8) at a flow rate of 10 g / h 3 Br. Introducing CF 3 During this phase of Br, SO in the reactor 2 The concentration was kept at 1% by contin...

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Abstract

The invention relates to a process for preparing an oxysulphide and fluorinated compound, which comprises reacting, in the presence of an organic solvent, at least one compound of formula Ea-X (I), in which Ea is a fluorine atom or a group preferably having from 1 to 10 carbon atoms, chosen from fluoroalkyls, perfluoroalkyls and fluoroalkenyls, and X is bromine, chlorine or iodine, and a sulphur oxide, said process being such that the concentration of sulphur oxide dissolved in the reaction medium is maintained at a value between 0.2% and 3% by weight. The use of an oxysulphide and fluorinated compound thus obtained for the synthesis of a sulphonimide compound of formula (Ea-SO2)2NH and of salts thereof (Ea-SO2)2NM, of a fluorinated sulphonic acid compound of formula Ea-SO2OH or of a fluorinated sulphonic anhydride compound of formula (Ea-SO2)2O is also described.

Description

technical field [0001] This invention relates to the preparation of oxysulfides and fluorinated compounds. More specifically, the present invention relates to an improved process which makes it possible to prepare fluorosulfinic acids, fluorosulfonic acids and bisfluorosulfimides and their salts, and also fluoroalkanesulfinic acids, fluoroalkanesulfonic Acids and difluoroalkane sulfonylimides and their salts. Background technique [0002] Perhaloalkanesulfonic acids and more specifically trifluoromethanesulfonic acids are used as catalysts or intermediates in organic synthesis. [0003] Methods for the synthesis of such oxysulfides and fluorinated organic compounds, and in particular perfluoromethanesulfinic acid in salified form, are already known. For example, document WO 2007 / 128893 describes the reaction of at least partially salified fluorocarboxylic acids and sulfur oxides in polar organic solvents. However, this reaction exhibits the disadvantage of being incomplet...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C313/04
CPCC07C313/04
Inventor D.勒弗朗V.达姆布林F.梅茨S.韦迪耶
Owner RHODIA OPERATIONS SAS
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