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Method for compounding 1-(2-Chloroethoxy)propane

A technology of propoxy ethyl chloride and n-propyl ether, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as high price, low product yield, cumbersome process, etc., and achieve production cost Low production rate, high product yield and simple process

Active Publication Date: 2016-02-24
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Tong Guotong discloses a preparation method of the herbicide pretilachlor intermediate 2-propoxychloroethane in the patent CN200810061878.0. The method uses bis(trichloromethyl)carbonate as the chlorinating agent instead of chlorinated ethylene chloride. Chlorinating agents such as sulfone, phosphorus oxychloride, and hydrogen chloride, under organic solvent conditions, use organic amines as catalysts to synthesize 2-propoxychloroethane. Due to the addition of organic solvents, the product must be distilled and purified, resulting in product yields The production rate is low, the energy consumption is high, the product quality is unstable, and there are many process steps. At the same time, the price of bis(trichloromethyl)carbonate (triphosgene for short) is relatively high, which is not conducive to industrialization.
[0004] The traditional synthesis method of 2-propoxychloroethane has problems such as low product yield, unstable quality, serious environmental pollution, cumbersome process and prominent safety hazards. Therefore, the development of efficient, safe and environmentally friendly 2-propoxychloroethane Ethane Production Process Gets Wide Attention

Method used

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  • Method for compounding 1-(2-Chloroethoxy)propane
  • Method for compounding 1-(2-Chloroethoxy)propane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 100g of ethylene glycol mono-n-propyl ether and 0.1g of dodecyltrimethylammonium chloride respectively and add them to the reaction vessel with a reflux condenser, add 125.66g of thionyl chloride to the constant pressure dropping funnel, and heat up to 35 ℃, start stirring, slowly add thionyl chloride dropwise to the reaction vessel, the reaction process releases sulfur dioxide and hydrogen chloride gas, control the rate of thionyl chloride addition to keep the temperature of the reaction solution at 55±5°C.

[0030] After the dropwise addition of thionyl chloride, gradually raise the temperature to 90°C according to the reaction gas release rate until no gas is released, and continue to keep warm for 2h to obtain the crude product; cool the crude product to 50°C, directly add solid sodium hydroxide and stir, and thoroughly dissolve the thionyl chloride Decompose to obtain 116.19 g of 2-propoxyl chloroethane. After testing, the chromatographic content of the product...

Embodiment 2

[0032] Take 100g of ethylene glycol mono-n-propyl ether and 0.3g of benzyltriethylammonium chloride into the reaction vessel with a reflux condenser, add 131.4g of thionyl chloride into the constant pressure dropping funnel, and heat up to 40°C. Start stirring, and slowly add thionyl chloride dropwise to the reaction vessel. During the reaction, sulfur dioxide and hydrogen chloride gas are released, and the rate of addition of thionyl chloride is controlled to keep the temperature of the reaction solution at 60±5°C.

[0033] After the dropwise addition of thionyl chloride is completed, gradually raise the temperature to 95°C according to the reaction gas release rate until no gas is released, and continue to keep warm for 3h to obtain the crude product; cool the crude product to 40°C, directly add solid sodium hydroxide and stir, and thoroughly dissolve the thionyl chloride Decompose to obtain 116.2 g of 2-propoxyl ethyl chloride. After testing, the chromatographic content of t...

Embodiment 3

[0035] Get 100g ethylene glycol mono-n-propyl ether, 0.5g methoxymethyltriphenylphosphine chloride respectively and add in the reaction vessel with reflux condenser, add 137.1g thionyl chloride into the constant pressure dropping funnel, heat up to At 45°C, start stirring, and slowly add thionyl chloride dropwise to the reaction vessel. During the reaction, sulfur dioxide and hydrogen chloride gas are released, and the rate of addition of thionyl chloride is controlled to keep the temperature of the reaction solution at 60±5°C.

[0036] After the dropwise addition of thionyl chloride, gradually raise the temperature to 100°C according to the reaction gas release rate until no gas is released, and continue to keep warm for 4h to obtain the crude product; cool the crude product to 30°C, directly add solid sodium hydroxide and stir, and thoroughly dissolve the thionyl chloride Decompose to obtain 116.08g of 2-propoxyl chloroethane. After testing, the chromatographic content of the...

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Abstract

The invention belongs to the technical field of organic syntheses, and in particular relates to a method for compounding 1-(2-Chloroethoxy)propane. The method comprises the steps of taking ethylene glycol monopropyl ether and thionyl chloride as main raw materials under the synergistic action of a phase transfer catalyst; controlling the reaction temperature by dripping the thionyl chloride; obtaining a crude product through temperature rising and temperature preservation; directly adding solid alkali to decompose and neutralize the excessive thionyl chloride after cooling; finally obtaining the 1-(2-Chloroethoxy)propane through filtering. Compared with the prior art, the efficiency of the catalyst is higher, the technology is simple and convenient, safety and reliability are realized, the yield of the product is high, the quality is stable, the product content is more than 99.2 percent, the yield is greater than 98.6 percent, the production cost is lower, and the method is particularly suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for synthesizing 2-propoxyethyl chloride. Background technique [0002] 2-Propoxyethyl chloride is one of the important raw materials for the preparation of the herbicide pretilachlor. As a low-toxicity, broad-spectrum and high-efficiency professional selective herbicide, it is widely used in the field of rice planting and has a broad market. The external demand is large. [0003] At present, the preparation of 2-propoxychloroethane mainly uses ethylene glycol mono-n-propyl ether as the starting material, and uses different chlorinating agents to chlorinate its hydroxyl group. Yang Jianping etc. (the synthetic method of 2-n-propoxyl ethyl chloride, Zhejiang chemical industry, 1999, the 30th volume, the 4th phase) are chlorination agent with ethylene glycol monopropyl ether and thionyl chloride, adopt composite catalyst, The content of the final pr...

Claims

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Application Information

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IPC IPC(8): C07C41/22C07C43/12
CPCC07C41/22C07C43/12
Inventor 张泰铭张善民毕义霞王荣海李文娟贾远超
Owner SHANDONG KAISHENG NEW MATERIALS
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