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Preparation method of 4-bromophenetole

A technology of bromophenethyl ether and p-bromophenol, which is applied in the field of organic compound preparation, can solve the problems of unfavorable economic benefits, difficulty in reducing costs, and many production equipments, and achieve the effects of improving product quality, reducing production costs, and convenient operation

Inactive Publication Date: 2010-12-15
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The usual production method of p-bromophenethyl ether is a diazotization reaction. Because the diazotization reaction needs to be carried out at low temperature, low-temperature freezing equipment is needed. The problems in this type of preparation method: 1. Because the diazotization reaction step needs to use expensive It can only be realized with a high-quality refrigeration pump. Therefore, this method has the problems of many production equipment and high cost, so it is difficult to reduce the cost.
2. Since the diazotization reaction step is an essential and very time-consuming and energy-consuming production step in the production of p-bromophenetole, this method has the problems of long production time and low production efficiency, which is not conducive to the economic benefits of enterprises improvement

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The preparation method of p-bromophenethyl ether comprises the following steps:

[0020] (1) Etherification reaction step: 10 moles of p-bromophenol, 200 moles of water, and 5 moles of diethyl sulfate are successively dropped into a 50-liter reactor with heating device, electric stirring, and thermometer, and heated to 35 React at ±2°C, keep this temperature, add 11 moles of potassium hydroxide continuously, keep the reaction for 1 hour after adding potassium hydroxide; stop heating, and the etherification reaction is terminated.

[0021] (2) Water washing step: put 600 moles of water in the mixed solution obtained after the etherification reaction, stir evenly, leave to stand for stratification, and separate the oil layer.

[0022] (3) Distillation step: the oil layer is introduced into steam to carry out steam distillation, even if the high-efficiency separation method that the fixed fraction is taken out by water vapor, the product obtained is the finished product of...

Embodiment 2

[0024] The preparation method of p-bromophenethyl ether comprises the following steps:

[0025] (1) Etherification reaction step: drop into 10 moles of p-bromophenol, 200 moles of water, and 5 moles of diethyl sulfate successively in a 50-liter reaction kettle with a heating device, electric stirring, and a thermometer, and heat to 40 moles while stirring. React at ±2°C, keep this temperature, add 11 moles of potassium hydroxide continuously, keep the reaction for 1 hour after adding potassium hydroxide; stop heating, and the etherification reaction is terminated.

[0026] (2) Water washing step: put 600 moles of water in the mixed solution obtained after the etherification reaction, stir evenly, leave to stand for stratification, and separate the oil layer.

[0027] (3) Distillation step: the oil layer is introduced into steam to carry out steam distillation, even if the high-efficiency separation method that the fixed fraction is taken out by water vapor, the product obtaine...

Embodiment 3

[0029] The preparation method of p-bromophenethyl ether comprises the following steps:

[0030] (1) Etherification reaction step: 10 moles of p-bromophenol, 200 moles of water, and 5 moles of diethyl sulfate are successively dropped into a 50-liter reactor with heating device, electric stirring, and thermometer, and heated to 45 React at ±2°C, keep this temperature, add 11 moles of potassium hydroxide continuously, keep the reaction for 1 hour after adding potassium hydroxide; stop heating, and the etherification reaction is terminated.

[0031] (2) Water washing step: put 600 moles of water in the mixed solution obtained after the etherification reaction, stir evenly, leave to stand for stratification, and separate the oil layer.

[0032] (3) Distillation step: the oil layer is introduced into steam to carry out steam distillation, even if the high-efficiency separation method that the fixed fraction is taken out by water vapor, the product obtained is the finished product of...

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Abstract

The invention relates to a preparation method of 4-bromophenetole. The method comprises (1) an etherification reaction step: putting p-bromophenol and diethyl sulfate into a reaction kettle, stirring, heating and continuously adding potassium hydroxide to react; (2) a washing step: adding water to the mixture after the etherification reaction, evenly stirring, standing still to delaminate and separate oily liquid; and (3) a distillation step: introducing vapor in the oily layer for vapor distillation to obtain the finished product of 4-bromophenetole. By using a vapor distillation technology and potassium hydroxide, the preparation method reduces the feeding amounts of diethyl sulfate and water, saves the cost of the raw materials, improves the product quality and enhances the 4-bromophenetole content to 99.5 percent.

Description

technical field [0001] The invention belongs to the field of preparation of organic compounds, in particular to a method for preparing p-bromophenetole. Background technique [0002] In the industrial production of chemiluminescent light, p-bromophenetole is more and more widely used as an important organic compound. The usual production method of p-bromophenethyl ether is a diazotization reaction. Because the diazotization reaction needs to be carried out at low temperature, low-temperature freezing equipment is needed. The problems in this type of preparation method: 1. Because the diazotization reaction step needs to use expensive Therefore, this method has the problems of many production equipments and high cost, so it is difficult to reduce the cost. 2. Since the diazotization reaction step is an essential and very time-consuming and energy-consuming production step in the production of p-bromophenetole, this method has the problems of long production time and low prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/225C07C41/16C07C41/42
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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