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Preparation method of 4-trifluoroethoxyl pyridine-N-oxide derivative

A technology of trifluoroethoxypyridine and trifluoroethoxy, applied in the field of synthesis of 4-trifluoroethoxypyridine-N-oxide derivatives, which can solve the problems of difficult preparation, expensive raw materials, and difficult availability

Inactive Publication Date: 2012-07-04
SHANGHAI SINOFLUORO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above methods, some raw materials (such as trifluoroethoxy ester) are difficult to prepare and are not easy to obtain; some raw materials are more expensive and are not suitable for large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Add 40ml of trifluoroethanol to the three-necked reaction flask, stir, add an appropriate amount of solid sodium hydroxide, and dissolve the solution, add 0.06ml of 4-nitropyridine-N-pyridine oxide, heat to reflux for 8h, reduce pressure, and evaporate the excess Trifluoroethanol, cooled, poured into a separatory funnel, added 20ml of water to dissolve the solid, extracted with 40ml*3 chloroform, dried with anhydrous magnesium sulfate, removed chloroform under reduced pressure, cooled, precipitated solid, filtered, washed , dried to obtain a crude product, which was recrystallized from ethyl acetate to obtain the product 4-(2,2,2-trifluoroethoxy)pyridine oxide.

Embodiment 2

[0011] Add 40ml of trifluoroethanol to the three-necked reaction flask, stir, add an appropriate amount of solid sodium hydroxide, after the solution is dissolved, add 0.06ml of 2,3-dimethyl-2-nitropyridine-N-pyridine oxide, and heat to reflux for 8h , reduced pressure, evaporated excess trifluoroethanol, cooled, poured into a separatory funnel, added 20ml of water to dissolve the solid, extracted with 40ml*3 chloroform, dried with anhydrous magnesium sulfate, removed chloroform under reduced pressure, Cooling, precipitation of solids, filtration, washing, drying to obtain a crude product, recrystallization with ethyl acetate to obtain the product 2,3-dimethyl-2-(2,2,2-trifluoroethoxy)pyridine oxide .

Embodiment 3

[0013] Add 40ml of trifluoroethanol to the three-necked reaction flask, stir, add an appropriate amount of solid sodium hydroxide, after the solution is dissolved, add 0.06ml of 2-methyl-3-chloro-4-nitropyridine-N-pyridine oxide, and heat to reflux 8h, reduce pressure, evaporate excess trifluoroethanol, cool, pour into a separatory funnel, add 20ml of water to dissolve the solid, extract with 40ml*3 chloroform, dry with anhydrous magnesium sulfate, remove chloroform under reduced pressure , cooled, precipitated solid, filtered, washed, dried to obtain a crude product, recrystallized with ethyl acetate to obtain the product 2-methyl-3-chloro-4-(2,2,2-trifluoroethoxy) Pyridine oxide.

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PUM

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Abstract

The invention provides a preparation method of a 4-trifluoroethoxyl pyridine-N-oxide derivative. In the method, 4-(2,2,2-trifluoroethoxyl)pyridine oxide, 2,3-dimethyl-2-(2,2,2-trifluoroethoxyl)pyridine oxide and 2-methyl-3-chlorin-4-(2,2,2-trifluoroethoxyl)pyridine oxide are prepared by taking a readily-available 4-nitro-N-pyridine oxide derivative and 2,2,2-trifluoroethanol as raw materials under the action of a strong alkali. The reaction conditions are mild, and operation is simple.

Description

technical field [0001] The invention relates to the field of fluorine chemical industry, in particular to a synthesis method of 4-trifluoroethoxypyridine-N-oxide derivatives. Background technique [0002] The synthetic method of 4-trifluoroethoxypyridine-N-oxide derivative mainly contains following several kinds: with 4-nitro-N-oxide pyridine derivative and various trifluoroethoxy esters (such as: trifluoro Ethoxysulfonate, trifluoroethoxybenzenesulfonate, etc.) as raw materials, hexamethylphosphoric triamide as solvent and sodium hydride reaction synthesis; with phenols and trifluoroiodoethane as starting materials, DMSO is a solvent, reacted under the action of catalyst potassium fluoride; reacts with halogenated benzene and sodium hydride, trifluoroethanol, with DMF as solvent; with nitropyridine and trifluoroethanol, potassium carbonate as raw material, acetonitrile as solvent, in The reaction is carried out under the catalysis of tetrabutylammonium bromide. In the abo...

Claims

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Application Information

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IPC IPC(8): C07D213/89
Inventor 闾肖波朱虹
Owner SHANGHAI SINOFLUORO SCI
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