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Production method of 2-propoxyethyl chloride

A technology for the production of propoxyethyl chloride, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of high energy consumption, low yield, cumbersome process steps, etc., and achieve catalytic efficiency High, simple process, stable quality effect

Inactive Publication Date: 2017-06-13
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a kind of production method of 2-propoxyl ethyl chloride, solve the problems of low yield, complex process steps and high energy consumption in the existing process, and have mild reaction conditions, simple process, The operation process is safe and reliable, and the purity and yield of the product are significantly improved

Method used

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  • Production method of 2-propoxyethyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The production method of 2-propoxyl ethyl chloride is as follows:

[0019] (1) Take by weighing 100g ethylene glycol mono-n-propyl ether and 0.1g triethylamine respectively, join it in the reaction vessel with reflux condenser, 116.41g thionyl chloride (content is 99.2%, sulfuryl chloride content 0.1%) into the constant pressure dropping funnel, heated up to 30°C, started stirring, and slowly added thionyl chloride dropwise to the reaction vessel, during the reaction, sulfur dioxide and hydrogen chloride gas were released, and the droplet rate of thionyl chloride was controlled. Acceleration, so that the temperature of the reaction solution is always maintained at 50 ° C;

[0020] (2) After the addition of thionyl chloride is completed, the temperature is gradually raised to 90°C according to the reaction gas release rate until no gas is released, and the crude product is obtained after the heat preservation is continued for 2 hours. After the crude product is cooled to...

Embodiment 2

[0022] The production method of 2-propoxyl ethyl chloride is as follows:

[0023] (1) Take by weighing 100g ethylene glycol mono-n-propyl ether and 0.2g triethylamine respectively, join it in the reaction vessel with reflux condenser, and 125.45g thionyl chloride (content is 99.0%, sulfuryl chloride content 0.3%) into the constant pressure dropping funnel, heated up to 35°C, started stirring, and slowly added thionyl chloride dropwise to the reaction vessel, sulfur dioxide and hydrogen chloride gas were released during the reaction, and the rate of addition of thionyl chloride was controlled , keep the temperature of the reaction solution at 60°C;

[0024] (2) After the addition of thionyl chloride is completed, the temperature is gradually raised to 95°C according to the reaction gas release rate until no gas is released, and the crude product is obtained after the heat preservation is continued for 3 hours. After the crude product is cooled to 40°C, a certain amount of lye i...

Embodiment 3

[0026] The synthetic technique of 2-propoxyl ethyl chloride is as follows:

[0027] (1) Take by weighing 100g ethylene glycol mono-n-propyl ether, 0.3g triethylamine respectively, join it in the reaction container with reflux condenser, 137.1g thionyl chloride (content is 98.3%, sulfuryl chloride content 0.5%) into the constant pressure dropping funnel, heated up to 35°C, started stirring, and slowly added thionyl chloride dropwise to the reaction vessel, during the reaction process, sulfur dioxide and hydrogen chloride gas were released, and the dropping rate of thionyl chloride was controlled , keep the temperature of the reaction solution at 55°C;

[0028] (2) After the dropwise addition of thionyl chloride is completed, the temperature is gradually raised to 95°C according to the reaction gas release rate until no gas is released, and the crude product is obtained after continuing to keep warm for 4 hours. After the crude product is cooled to 40°C, a certain amount of lye ...

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Abstract

The invention relates to a production method of 2-propoxyethyl chloride and belongs to the technical field of fine chemical intermediate organic synthesis. The synthesis process comprises the following steps: preparing a crude product by taking ethylene glycol monopropyl ether and excessive sulfoxide chloride as main raw materials and adopting an efficient catalyst through heating and heat preservation, wherein the reaction rate is controlled by dropwise adding sulfoxide chloride; and performing neutralization, hydrolysis, and liquid separation after standingto obtain 2-propoxyethyl chloride. Compared with the existing process, the synthesis process has the advantages that the catalyst has higher catalytic efficiency and is cheap and easily available; the technological process is simple and convenient; the catalyst used in the existing process and hydrochloric acid in the crude product form a complex easily, so that the product has precipitates and the product yield is influenced; and the crude product prepared by the catalyst is clear and transparent, the product can be obtained without water washing, the quality is stable, the product content reaches above 99.5 percent, the yield is more than 99.0 percent, the production cost is lower, and the synthesis process is particularly suitable for industrialized production.

Description

technical field [0001] The invention relates to a production method of 2-propoxyethyl chloride, which belongs to the technical field of organic synthesis of fine chemical intermediates. Background technique [0002] Pretilachlor is a low-toxic, high-efficiency early broad-spectrum paddy field selective bud stage herbicide, which is widely used in the field of rice planting, has a broad market, and has a large demand at home and abroad, while 2-propoxychloroethane is One of the important raw materials for the preparation of the herbicide pretilachlor. [0003] At present, the method for industrially producing 2-propoxyl ethyl chloride is mainly to use ethylene glycol mono-n-propyl ether as the starting material, and adopt different chlorinating agents to chlorinate its hydroxy groups, as in "Zhejiang Chemical Industry" in 1999, 30 (4) The publicly published "synthetic method of 2-n-propoxyl ethyl chloride", which takes ethylene glycol monopropyl ether as the starting materia...

Claims

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Application Information

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IPC IPC(8): C07C41/22C07C43/12
CPCC07C41/22C07C43/12
Inventor 石余飞薛居强张泰铭王军王荣海李光辉黄桂青韩楠楠
Owner SHANDONG KAISHENG NEW MATERIALS
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