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Preparation of N-methy-3,5-ditrifluo-aniline

A technology of trifluoromethylbenzylamine and methyl, which is applied in the field of preparing N-methyl-3 by catalytic hydrogenation of metals, which can solve the problems of high preparation cost, low reaction yield, high price of sodium cyanoborohydride, etc. problem, to achieve the effect of low cost and high yield

Inactive Publication Date: 2007-07-25
LYNCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

Because the reaction yield is low (52%) and sodium cyanoborohydride is expensive, the preparation cost of N-methyl-3,5-bistrifluoromethylbenzylamine is higher

Method used

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  • Preparation of N-methy-3,5-ditrifluo-aniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0010] Embodiment: the preparation of N-methyl-3,5-bistrifluoromethylbenzylamine

[0011] N-methyl-3,5-bistrifluoromethylbenzylamine can be prepared through the following synthetic route.

[0012]

[0013] Add 50g of 3,5-bistrifluoromethylbenzaldehyde (II) and 50g of tetrahydrofuran into a 1000ml four-necked flask equipped with a stirrer, a thermometer, and a low-temperature cold water bath, cool down to 0-5°C, keep this temperature, and Under vigorous stirring, a solution of 50 g of methylamine hydrochloride dissolved in 250 ml of methanol and 75 ml of triethylamine were successively added dropwise, and after the dropwise reaction, the reaction solution was transferred to a 1000 ml autoclave. Under stirring, add R-Ni catalyst 2.5g in autoclave, use N 2 Replace the air in the kettle, heat the temperature inside the kettle to 80°C, and slowly fill the kettle with H 2 , until the kettle pressure was 4MPa, after continuing to react at this temperature for 6h, the catalyst R-...

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PUM

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Abstract

Production of N-methyl-3,5-bistriflumethylaniline is carried out by oximation reacting 3,5-bistriflutoluyl aldehyde with methylamine hydrochloride, catalyzing and reducing the products. It yields more and is cheap.

Description

technical field [0001] The invention relates to a method for preparing N-methyl-3,5-bistrifluoromethylbenzylamine, in particular to the preparation of N-methyl-3,5-bistrifluoromethylbenzylamine by metal catalytic hydrogenation Methods. Background technique [0002] N-methyl-3,5-bistrifluoromethylbenzylamine is a new type of pharmaceutical intermediate, which can be used to prepare fungicides. Prior art such as patent GB 2282 807 A has disclosed the synthesis method of N-methyl-3,5-bistrifluoromethylbenzylamine, wherein by 3,5-bistrifluoromethylbenzaldehyde as raw material, through After oximation with methylamine hydrochloride, sodium cyanoborohydride (NaBH 3 CN) is prepared by reduction. Due to the low reaction yield (52%) and the high price of sodium cyanoborohydride, the preparation cost of N-methyl-3,5-bistrifluoromethylbenzylamine is relatively high. Contents of the invention [0003] The object of the present invention is to provide a method for the preparation o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/68C07C211/29
Inventor 陈荣业李振威
Owner LYNCHEM
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