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Synthesis process of 2-propoxyethyl chloride

A technology for the synthesis of propoxy ethyl chloride and the synthesis process, which is applied in the field of synthesis of 2-propoxy ethyl chloride, can solve the problems of cumbersome process steps, low yield, high energy consumption, etc., and achieve high catalytic efficiency and high production efficiency. low cost effect

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

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Problems solved by technology

[0004] The purpose of the present invention is to provide a synthesis process of 2-propoxyl ethyl chloride, which solves the problems of low yield, cumbersome process steps and high energy consumption in the existing process, and has the advantages of 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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  • Synthesis process of 2-propoxyethyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The synthetic technique of 2-propoxyl ethyl chloride is as follows:

[0019] (1) Weigh 100g of ethylene glycol mono-n-propyl ether and 0.1g of N,N-dimethylaniline respectively, and add them to a reaction vessel with a reflux condenser, and 114.83g of thionyl chloride (with a content of 99.2 %, the content of sulfuryl chloride is 0.1%) into the constant pressure dropping funnel, the temperature is raised to 35° C., the stirring is started, and the thionyl chloride is slowly added dropwise to the reaction vessel. During the reaction, sulfur dioxide and hydrogen chloride gas are released to control chlorine The drop rate of sulfoxide keeps the temperature of the reaction solution at 55±5°C;

[0020] (2) After the dropwise 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 1 hour. After the cr...

Embodiment 2

[0022] The synthetic technique of 2-propoxyl ethyl chloride is as follows:

[0023] (1) Weigh 100g of ethylene glycol mono-n-propyl ether and 0.2g of N,N-dimethylaniline respectively, and add them to a reaction vessel with a reflux condenser, and 115.40g of thionyl chloride (with a content of 99.0 %, the content of sulfuryl chloride is 0.3%) into the constant pressure dropping funnel, the temperature is raised to 40° C., the stirring is started, and the thionyl chloride is slowly added dropwise to the reaction vessel. During the reaction, sulfur dioxide and hydrogen chloride gas are released to control chlorine Increase the sulfoxide drop rate to keep the temperature of the reaction solution at 60±5°C;

[0024] (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 the heat preservation is continued for 1 hour. Afte...

Embodiment 3

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

[0027] (1) Weigh 100g of ethylene glycol mono-n-propyl ether and 0.3g of N,N-dimethylaniline respectively, and add them to a reaction vessel with a reflux condenser, and 115.97g of thionyl chloride (with a content of 99.3 %, the content of sulfuryl chloride is 0.5%) into the constant pressure dropping funnel, the temperature is raised to 35°C, the stirring is started, and the thionyl chloride is slowly added dropwise to the reaction vessel. During the reaction, sulfur dioxide and hydrogen chloride gas are released to control the chlorine Increase the sulfoxide drop rate to keep the temperature of the reaction solution at 60±5°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 the heat preservation is continued for 1 hour. Af...

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Abstract

The invention relates to a synthesis process 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 standing to obtain 2-propoxyethyl chloride. Compared with the existing process, the synthesis process has the advantages that the catalyst has higher catalytic efficiency; and the existing process needs 0.1 to 0.2 mol of excessive sulfoxide chloride, but the catalyst only needs 0.01 mol of excessive sulfoxide chloride, so fewer waste water and waste residues are generated when the crude product is treated, 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 suitable for industrialized production.

Description

technical field [0001] The invention relates to a synthesis process 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 herbicide, which is widely used in the field of rice planting, has a broad market, and has a large demand at home and abroad. 2-Propoxychloroethane is the preparation One of the important raw materials 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 material, thionyl chlor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/12C07C41/22C07C41/34
CPCC07C41/22C07C41/34C07C43/12
Inventor 石余飞张泰铭韩楠楠王荣海薛居强王军李光辉黄桂青
Owner SHANDONG KAISHENG NEW MATERIALS
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