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A kind of preparation method of 2-chloroethoxy-2-ethoxydiethanol

A technology of ethoxydiethanol and chloroethoxy is applied in the preparation of ether from alkylene oxide, ether preparation, organic chemistry, etc., and can solve the problems of poor selectivity of the preparation method, unfavorable industrial production, and difficult preparation, and achieve technological progress. Significant, three-waste treatment cost reduction and pollution reduction effect

Active Publication Date: 2016-01-20
SHANGHAI CHEMPARTNER CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] In view of the above-mentioned defects in the prior art, the technical problem to be solved by this invention is to provide a kind of preparation method of 2-chloroethoxy-2-ethoxydiethanol, which described method will solve the problems of the prior art The preparation method has poor selectivity, low yield, difficult preparation and technical problems that are unfavorable for industrialized production

Method used

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  • A kind of preparation method of 2-chloroethoxy-2-ethoxydiethanol
  • A kind of preparation method of 2-chloroethoxy-2-ethoxydiethanol
  • A kind of preparation method of 2-chloroethoxy-2-ethoxydiethanol

Examples

Experimental program
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Effect test

Embodiment 1

[0038] In a 1000ml three-necked flask, add 685g (8.5mol) of 2-chloroethanol, 3.3g of catalyst, start the stirrer and heater, and raise the temperature to 40°C (in order to maintain the reaction temperature at 40-50°C, the ethylene oxide must be controlled Introduce speed, if necessary, use a water bath to control the temperature), slowly inject 44g of ethylene oxide into the flask, and the introductory time is 1.5-2h. In order to make the reaction complete, after passing through ethylene oxide, continue to stir the reaction for 0.5h. After stirring, heat up, remove excess 2-chloroethanol under reduced pressure, vacuum degree 0.075mPa (water flushing pump), final desolvation temperature 105°C, collect about 592g of 2-chloroethanol (can be recycled), flask The material mainly based on the intermediate product 2-chloroethoxyethanol is obtained.

[0039] Cool the material in the three-necked flask to 45-50°C, add 0.7g of boron trifluoride ether, and pass in 46.2g (1.05mol) of eth...

Embodiment 2

[0042] In a 1000ml three-necked flask, add 685g of 2-chloroethanol (592g+93g new for recycling) (8.5mol), 3.3g of catalyst, start the stirrer and heater, and heat up to 40°C (in order to keep the reaction temperature at 40-50 ℃, to control the speed of ethylene oxide feeding, if necessary, use a water bath to control the temperature), slowly feed 44g of ethylene oxide into the flask, and the feeding time is 1.5-2h. In order to make the reaction complete, after passing through ethylene oxide, continue to stir the reaction for 0.5h. After the stirring is over, start to heat up, remove excess 2-chloroethanol under reduced pressure, the vacuum degree is 0.075mPa (water flushing pump), the final desolvation temperature is 105°C, and about 587g of 2-chloroethanol is collected, which can be used mechanically. Inside is the material mainly containing the intermediate product 2-chloroethoxyethanol.

[0043] Cool the material in the three-necked flask to 45-50°C, add 0.7g of boron trif...

Embodiment 3

[0045] The amount of catalyst used in Example 2 was reduced to 0.3% of the total amount of materials, and the feeding ratio and reaction conditions were the same as in Example 2. After rectification, 116.7 g of the product was obtained, with a gas phase content of 97.6% and a total yield of 69.2%.

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Abstract

The invention discloses a preparation method of 2-chloroethoxy-2-ethyoxylethanol. The preparation method comprises the steps: with 2-chloroethoxy and ethylene oxide as raw materials, performing a reaction in the presence of a catalyst to firstly obtain 2-ethyoxylethanol, removing the remaining solvent, namely a reactant 2-chlorohydrin, making the 2-ethyoxylethanol continuously react with the re-added ethylene oxide to obtain a target product 2-chloroethoxy-2-ethyoxylethanol. The preparation method has the advantages of being easy to operate during reaction, mild in system, less in side reactions, high in content and yield of products, and less in pollutants generated during the reaction.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a pharmaceutical intermediate 2-chloroethoxy-2-ethoxydiethanol, in particular to a preparation method of 2-chloroethoxy-2-ethoxydiethanol. Background technique [0002] 2-Chloroethoxy-2-ethoxydiethanol, referred to as CEEE, is a colorless transparent liquid with a CAS registration number of [5197-62-6] and a structural formula of: [0003] [0004] 2-Chloroethoxy-2-ethoxydiethanol, as an intermediate of PranedipineTartrate and LJP-920, is an important intermediate of pharmaceutical and chemical industry. [0005] Its synthesis method mainly contains following three kinds: [0006] A: 2-chloroethoxy-2-ethoxydiethanol is prepared by direct etherification reaction of triethylene glycol and HCl. The synthetic route is as follows: [0007] [0008] The raw materials of this method are easy to obtain, but there are many side reactions, poor selectivity, low yield an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/12C07C41/03
CPCC07C41/03C07C43/11C07C43/137
Inventor 蒋继波马鹏韩生叶冯英于飞刘程陈永悦刘亚锋刘凡黄奇何慧红祝俊
Owner SHANGHAI CHEMPARTNER CO LTD
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