Method for synthesizing bromoethyl acetate

A technology of ethyl bromoacetate and a synthetic method, applied in the synthesis field of ethyl bromoacetate, can solve problems such as patent documents that have not yet been found, and achieve the effects of easy control, reasonable and feasible process, and low cost

Inactive Publication Date: 2010-11-24
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] By searching, no patent documents related to the present invention have been found

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A kind of synthetic method of ethyl bromoacetate, concrete operation steps are as follows.

[0024] (1) Bromination: Add 70 g of acetic acid and 20 g of red phosphorus in a reaction flask with a stirrer, reflux condenser, dropping funnel, and thermometer, heat to 70° C., start to add 168 g of bromine dropwise, and finish adding in 24 hours. Add 3-5 liters of water, heat to reflux for 2 hours, filter after cooling, then distill off hydrogen bromide and water before 140°C, and pour the residue into an enamel dish to crystallize bromoacetic acid, about 140g.

[0025] (2) Esterification: add bromoacetic acid, 72g ethanol, 5ml vitriol oil that last step makes in the reaction bottle that has agitator, reflux condenser, water separator, thermometer, heat and carry out esterification dehydration, when water separation When the amount of water separated in the vessel remained substantially constant (19ml), the reaction was complete.

[0026] (3) Neutralization and washing with ...

Embodiment 2

[0029] A kind of synthetic method of ethyl bromoacetate, concrete operation steps are as follows.

[0030] (1) Bromination: Add 72g of acetic acid and 20g of red phosphorus in a reaction flask with a stirrer, reflux condenser, dropping funnel, and thermometer, heat to 70°C, start to add 170g of bromine dropwise, and finish adding in 22 hours. Add 3-5 liters of water and heat to reflux for 2 hours, filter after cooling, then distill off the hydrogen bromide and water before 140°C, and pour the residue into an enamel dish to crystallize into bromoacetic acid, about 139g.

[0031] (2) Esterification: add bromoacetic acid, 78g ethanol, 5ml vitriol oil that last step makes in the reaction bottle that has agitator, reflux condenser, water separator, thermometer, heat and carry out esterification dehydration, when water separation When the amount of water separated in the vessel was substantially constant (18.5ml), the reaction was complete.

[0032] (3) Neutralization and washing w...

Embodiment 3

[0035] A kind of synthetic method of ethyl bromoacetate, concrete operation steps are as follows.

[0036] Steps:

[0037] (1) Bromination: Add 75g of acetic acid and 20g of red phosphorus in a reaction flask with a stirrer, reflux condenser, dropping funnel, and thermometer, heat to 70°C, start adding 162g of bromine dropwise, and finish adding in 22.5 hours. Add 3-5 liters of water and heat to reflux for 2 hours, filter after cooling, then distill off hydrogen bromide and water before 140°C, and pour the residue into an enamel dish to crystallize into bromoacetic acid, about 140g.

[0038] (2) Esterification: add the bromoacetic acid, 80g ethanol, 5ml vitriol oil that last step makes in the reaction bottle that has agitator, reflux condenser, water separator, thermometer, heat and carry out esterification dehydration, when water separation When the amount of water separated in the vessel was substantially constant (17.5ml), the reaction was complete.

[0039] (3) Neutraliz...

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PUM

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Abstract

The invention relates to a method for synthesizing bromoethyl acetate, which comprises the following steps of: performing bromination reaction of bromine and acetic acid under the catalysis of red phosphorus to prepare bromoacetic acid, and performing esterification reaction of the bromoacetic acid and ethanol under the catalysis of sulfuric acid to prepare the bromoethyl acetate. In the method, the bromination reaction and the esterification reaction in a synthetic process are fundamental reactions in organic synthesis, and are convenient to operate and easy to master; and the process has the advantages of reasonability, feasibility, low cost and easy realization of industrial production, and because the provided bromoethyl acetate is an important organic synthesis raw material, the bromoethyl acetate is used as a synthetic intermediate specially for pesticides, herbicides and bactericides.

Description

technical field [0001] The invention belongs to the field of fine chemical industry and relates to a synthesis method of ethyl bromoacetate. Background technique [0002] Ethyl bromoacetate is a colorless and clear liquid, which is miscible with ethanol, ether and benzene. It is an important fine chemical and has a wide range of applications. It can be used as a special synthetic intermediate for medicine, pesticide and herbicide, and is an important raw material for organic synthesis. [0003] By searching, no patent documents related to the present invention have been found yet. Contents of the invention [0004] The object of the invention is to overcome the weak points of the prior art, and a kind of synthetic method of ethyl bromoacetate is provided. [0005] The technical scheme that the present invention realizes purpose is: [0006] A kind of synthetic method of ethyl bromoacetate is that bromine and acetic acid carry out bromination reaction under the catalysis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/63C07C67/08
Inventor 张序红
Owner TIANJIN CHEM REAGENT RES INST
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