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

A technology of trifluoromethylbenzylamine and trifluoromethylbenzaldehyde, which is applied in the field of preparing N-methyl-3 by metal catalytic hydrogenation, can solve the problem of low reaction yield, high preparation cost and cyanoborohydrogenation Sodium is expensive and other problems, to achieve the effect of high yield and low cost

Inactive Publication Date: 2006-03-15
LYNCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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 1282 807A has disclosed the synthetic method of N-methyl-3,5-bistrifluoromethylbenzylamine, wherein by 3,5-bistrifluoromethylbenzaldehyde is raw material, through and After methylamine hydrochloride was oximated, and then treated with 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 metho...

Claims

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Application Information

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IPC IPC(8): C07C211/29C07C209/68
Inventor 陈荣业李振威
Owner LYNCHEM
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