The method for synthesizing 2-propoxyl ethyl chloride

A technology of propoxyl 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 low product yield, high price, cumbersome process, etc., and achieve product yield The effect of high efficiency, low production cost and simple process

Active Publication Date: 2018-01-12
SHANDONG KAISHENG NEW MATERIALS
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  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • The method for synthesizing 2-propoxyl ethyl chloride
  • The method for synthesizing 2-propoxyl ethyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

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

[0030] After the addition of thionyl chloride is completed, gradually increase the temperature to 90°C according to the reaction gas evolution rate, until no gas is released, continue to keep the temperature for 2h to obtain the crude product; the crude product is cooled to 50°C, directly add solid sodium hydroxide and stir to thoroughly remove the thionyl chloride After decomposition, 116.19 g of 2-propoxychloroethane was obtained. After testing, the chromatographic content of the product was 99....

Embodiment 2

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

[0033] After the addition of thionyl chloride is completed, gradually increase the temperature to 95°C according to the rate of reaction gas evolution, until there is no gas evolution, continue to keep the temperature for 3h to obtain the crude product; the crude product is cooled to 40°C, directly add solid sodium hydroxide and stir to thoroughly remove the thionyl chloride After decomposition, 116.2 g of 2-propoxy chloroethane was obtained. After testing,...

Embodiment 3

[0035] Take 100g of ethylene glycol mono-n-propyl ether and 0.5g of methoxymethyl triphenylphosphine chloride into the reaction vessel with reflux condenser, add 137.1g of thionyl chloride into the constant pressure dropping funnel, and heat to Turn on the stirring at 45°C and slowly add thionyl chloride dropwise to the reaction vessel. Sulfur dioxide and hydrogen chloride gas are released during the reaction. The thionyl chloride dropping rate is controlled to keep the temperature of the reaction solution at 60±5°C.

[0036] After the addition of thionyl chloride is completed, gradually increase the temperature to 100°C according to the rate of reaction gas evolution, until no gas is released, continue to keep the temperature for 4h to obtain the crude product; the crude product is cooled to 30°C, directly add solid sodium hydroxide and stir to thoroughly remove the thionyl chloride After decomposition, 116.08 g of 2-propoxy chloroethane was obtained. After testing, the chromatog...

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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 specifically relates to a method for synthesizing 2-propoxychloroethane. Background technique [0002] 2-Propoxychloroethane is one of the important raw materials for the preparation of the herbicide pretilachlor. As a low-toxic, broad-spectrum, high-efficiency professional selective herbicide, it is widely used in the field of rice cultivation and has a broad market. Large external demand. [0003] At present, the preparation of 2-propoxy chloroethane mainly uses ethylene glycol mono-n-propyl ether as the starting material and uses different chlorinating agents to chlorinate its hydroxyl group. Yang Jianping et al. (Synthetic method of 2-n-propoxy chloroethane, Zhejiang Chemical Industry, 1999, Volume 30, Issue 4) used ethylene glycol monopropyl ether and thionyl chloride as chlorinating agents, using a composite catalyst, The final product content can reach 98.1%, and the yield is 97%....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/22C07C43/12
CPCC07C41/22C07C43/12
Inventor 贾远超张泰铭马团芝毕义霞张善民李文娟王鑫海贾亚非
Owner SHANDONG KAISHENG NEW MATERIALS
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