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Method for preparing tetrabutyl ammonium bromide

A technology of tetrabutylammonium bromide and bromobutane, which is applied in the field of organic compound preparation, can solve the problem of low product yield, achieve the effect of increasing product yield, improving economic and social benefits

Inactive Publication Date: 2011-04-20
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the yield of the synthesized product is not high without increasing advanced equipment and increasing the technical requirements of operators

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) synthetic reaction of tetrabutylammonium bromide

[0018] Into a 1000 ml reactor with heating device, electric stirring, thermometer and water circulation condenser, put 200 grams of tri-n-butylamine, 200 grams of bromobutane, 200 grams of solvent acetonitrile, stir and heat to slow reflux, constant temperature React for 22-24 hours;

[0019] (2) make tetrabutylammonium bromide crude product

[0020] Distill the mixture obtained after the reaction under normal pressure, recover acetonitrile and excess bromobutane, heat to 100°C, remove the remaining acetonitrile and bromobutane under reduced pressure, and the obtained light yellow transparent liquid is crude tetrabutylammonium bromide ;

[0021] (3) refined

[0022] Add 150 grams of ethyl acetate to the crude product of tetrabutylammonium bromide, heat to reflux and keep it warm for 0.5 hours, then cool and crystallize, filter, and decompress the product at 50°C, keep the vacuum at 30-35mmHg, remove the remaining...

Embodiment 2

[0024] (1) synthetic reaction of tetrabutylammonium bromide

[0025] Put 200 grams of tri-n-butylamine, 200 grams of bromobutylamine, and 250 grams of solvent acetonitrile into a 1000-milliliter reactor equipped with a heating device, electric stirring, thermometer, and water circulation condenser, stir and heat to slow reflux, and react at a constant temperature 22-24 hours;

[0026] (2) make tetrabutylammonium bromide crude product

[0027] Distill the mixture obtained after the reaction under normal pressure, recover acetonitrile and excess bromobutane, heat to 100°C, remove the remaining acetonitrile and bromobutane under reduced pressure, and the obtained light yellow transparent liquid is crude tetrabutylammonium bromide ;

[0028] (3) refined

[0029] Add 150 grams of ethyl acetate to the crude product of tetrabutylammonium bromide, heat to reflux and keep it warm for 0.5 hours, then cool and crystallize, filter, and decompress the product at 50°C, keep the vacuum at...

Embodiment 3

[0031] (1) synthetic reaction of tetrabutylammonium bromide

[0032] Into a 1000 ml reactor with heating device, electric stirring, thermometer, water circulation condenser, drop 200 grams of tri-n-butylamine, 200 grams of bromobutane, 300 grams of solvent acetonitrile, stir and heat to slow reflux, constant temperature React for 22-24 hours;

[0033] (2) make tetrabutylammonium bromide crude product

[0034] Distill the mixture obtained after the reaction under normal pressure, recover acetonitrile and excess bromobutane, heat to 100°C, remove the remaining acetonitrile and bromobutane under reduced pressure, and the obtained light yellow transparent liquid is crude tetrabutylammonium bromide ;

[0035] (3) refined

[0036] Add 150 grams of ethyl acetate to the crude product of tetrabutylammonium bromide, heat to reflux and keep it warm for 0.5 hours, then cool and crystallize, filter, and decompress the product at 50°C, keep the vacuum at 30-35mmHg, remove the remaining ...

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PUM

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Abstract

The invention relates to a method for preparing tetrabutyl ammonium bromide, which is characterized by comprising the following steps of: (1) performing the synthetic reaction of the tetrabutyl ammonium bromide; (2) preparing a crude product of the tetrabutyl ammonium bromide; and (3) refining. The method improves the product yield, meets the requirement of the market and improves the economic benefit and the social benefit of enterprises.

Description

technical field [0001] The invention relates to the field of preparation methods of organic compounds, in particular to a preparation method of tetrabutylammonium bromide. Background technique [0002] Tetrabutylammonium bromide is a common chemical product in the market. It is an ion-pairing reagent and is used in the synthesis of bahamicillin and sultacillin. It is also an effective phase transfer catalyst. At present, the yield of the synthesized product is not high without increasing the advanced equipment and increasing the technical requirements of the operators. Contents of the invention [0003] The object of the invention is to overcome the deficiencies in the prior art, and a kind of preparation method of tetrabutylammonium bromide is provided. [0004] In order to achieve the above object, the present invention adopts the following technical solutions: [0005] (1) synthetic reaction of tetrabutylammonium bromide [0006] Mix tri-n-butylamine, bromobutane and...

Claims

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Application Information

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IPC IPC(8): C07C211/63C07C209/12
Inventor 徐博刚
Owner TIANJIN CHEM REAGENT RES INST
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