Method for preparing organic chlorofluoro compounds from organic polychlorinated compounds

A technology of organic chlorofluoro compounds and chlorine compounds, which is applied in the field of preparation of organic fluorochloro compounds, can solve problems such as low reaction yield, low selectivity, and many impurities, and achieve simple preparation process, improved selectivity, and selectivity high effect

Inactive Publication Date: 2010-03-17
NANJING NO 1 PESTICIDE GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the traditional method is used to prepare chlorofluoro compounds, the selectivity is not high, and the depth of fluorination cannot be well controlled. The resulting compound is a mixture of monofluoro chloro compounds, difluoro chloro compounds or polyfluoro chloro compounds. Since these substances have similar properties As a result, the reaction yield is low, the impurities are many, and the separation is difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1、2

[0013] Embodiment 1,2, the synthesis of 3-difluoro-5-chloropyridine:

[0014] Weigh 36.5 grams (0.2mol) of 2,3,5-trichloropyridine, 84 grams of dimethylsulfoxide, 27.84 grams (0.48mol) of anhydrous potassium fluoride, 0.7 grams of triethylbenzyl ammonium chloride, 420 gram of n-hexane, put it into a dry 1000ml autoclave, heat up to 150°C for 6 hours, take out the reaction solution after dropping to normal temperature, and move it to a separatory funnel for layering. The purity measured by gas chromatography was 96.1%, and the bottom liquid was distilled to obtain 89 grams of recovered liquid. The content of the target substance was 5.3% and the raw material was 1.2% as measured by gas chromatography. The reaction yield is 95%.

Embodiment 2

[0015] The synthesis of embodiment 2,3-chloro-4-fluoronitrobenzene

[0016] Take by weighing 38.4 grams (0.2mol) 3,4-dichloronitrobenzene, 70 grams of dimethyl sulfoxide, 13.9 grams (0.24mol) of anhydrous potassium fluoride, 0.7 gram of triethylbenzyl ammonium chloride, 490 gram of n-hexane, put it into a dry 1000ml autoclave, raise the temperature to 130°C for 5 hours, take out the reaction solution after dropping to normal temperature, and move it to a separatory funnel for layering. The purity measured by gas chromatography was 95.3%, and the bottom liquid was distilled to obtain 72 grams of recovered liquid. The content of the target substance was 6.4% and the raw material was 1.9% as measured by gas chromatography. The reaction yield is 94%.

Embodiment 3

[0017] Synthesis of embodiment 3,2-fluoro-3,6-dichloropyridine

[0018] Weigh 36.5 grams (0.2mol) of 2,3,6-trichloropyridine, 51.2 grams of dimethylsulfoxide, 12.8 grams (0.22mol) of anhydrous potassium fluoride, 0.7 grams of triethylbenzyl ammonium chloride, 307.2 gram of n-hexane, put it into a dry 1000ml autoclave, heat up to 160°C and react for 15 hours, after dropping to normal temperature, take out the reaction solution and move it to a separatory funnel for layering. The purity measured by gas chromatography was 91.5%, and the lower layer liquid was distilled to obtain 49.6 grams of recovered liquid. The content of the target substance and the raw material were 2.8% as measured by gas chromatography. The reaction yield was 89%.

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Abstract

The invention discloses a method for preparing organic chlorofluoro compounds from organic polychlorinated compounds, which is realized by the following steps: adding organic polychlorinated compoundsand an alkali metal fluridizer to a mixed polar and nonpolar solvent, and carrying out the substitution reaction at 100-200 DEG C to prepare the organic chlorofluoro compounds. The method can controlthe fluorating depth with high selectivity so as to purposefully control the quantity of chlorine atoms substituted by fluorine in the organic polychlorinated compounds, so that not all chlorine atoms can be substituted. The method has the advantages of simple preparation process, high selectivity and high yield, and is suitable for large-scale commercial production.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and in particular relates to a preparation method of organic chlorofluoro compounds. Background technique [0002] Since the advent of Freon in the 1930s, organic chlorofluoro compounds have been widely used because of their unique physical and chemical properties. Especially in recent years, the application of fluorine-containing organic compounds in the fields of pesticides and medicines is in the ascendant. A method for preparing organic fluorine chlorides is to firstly prepare chlorides through chlorination reaction, and then synthesize target compounds through halogen exchange reaction with fluorinating agent at a certain temperature. The selectivity of the traditional method to prepare chlorofluoro compounds is not high, and the depth of fluorination cannot be well controlled. The resulting compound is a mixture of chlorofluoro compounds, chlorofluoro compounds or polyfluoro chloro co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07B39/00C07D213/61C07C205/12C07C201/12C07D239/30C07C17/20
Inventor 薛谊江涛蒋剑华王述刚徐强
Owner NANJING NO 1 PESTICIDE GRP
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