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Improved method for preparing glycine ethyl ester hydrochloride

A technology of glycine ethyl ester hydrochloride and glycine, which is applied in the field of preparation of glycine ethyl ester hydrochloride, can solve the problems of high price of triethyl orthoformate, complicated separation process, increased production cost, etc., and reduce the amount of leftovers to be processed and waste salt, the effect of reducing the content of glycine hydrochloride and reducing energy consumption

Active Publication Date: 2018-09-04
江苏优普生物化学科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the synthesis process, triethyl orthoformate may also react with ethanol to produce products such as ethyl acetate. There are many by-products, the separation process is complicated, and the price of triethyl orthoformate is relatively high, which increases the production cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 2000L glass-lined esterification kettle with a reflux device, add 1000 kg of absolute ethanol (99.75%, 21.68kmol), start stirring, add 400 kg of glycine (98.5%, 5.2kmol), seal the lid of the kettle, and pass it into a dry Hydrogen chloride gas, control the flow of hydrogen chloride to 30~80Nm 3 / h, when the temperature in the kettle rises to 40°C, turn on the jacket cooling water, control the temperature at 65~78°C, reflux reaction, until most of the kettle is dissolved, adjust the flow rate of hydrogen chloride to 10~30Nm 3 / h, until the material in the kettle is completely dissolved and clarified, stop passing hydrogen chloride. The esterification kettle was jacketed with steam, refluxed at 75~80°C for 1 hour, and discharged into a 2000L glass-lined crystallization kettle. Cool to 25°C, keep warm for one hour, discharge and centrifuge, dry the filter cake, detect the content of glycine ethyl ester hydrochloride 96.7% (dry basis, the same below), and the content ...

Embodiment 2

[0020] As in Example 1, the feed is esterified, the temperature is lowered to 16°C during crystallization, the temperature is kept for one hour, the material is discharged and centrifuged, the filter cake is dried, and the content of glycine ethyl ester hydrochloride is 95.3%, and the content of glycine hydrochloride is 4.7%. After washing twice with ethanol, it was detected that the content of glycine ethyl ester hydrochloride was 97.6%, and the content of glycine hydrochloride was 1.8%. Wash again, detect glycine ethyl ester hydrochloride content 98.1%, glycine hydrochloride content 1.1%. Vacuum dried to obtain 556.9 kg of product, yield 74.55%.

Embodiment 3

[0022] In a 2000L glass-lined esterification kettle with a reflux device, add 1200 kg of absolute ethanol (99.75%, 26.02kmol), start stirring, add 300 kg of glycine (98.5%, 3.94kmol), seal the lid of the kettle, and pass it into a dry Hydrogen chloride gas, control the flow of hydrogen chloride to 30~80Nm 3 / h, when the temperature in the kettle rises to 40°C, turn on the jacket cooling water, control the temperature at 65~78°C, reflux reaction, until most of the kettle is dissolved, adjust the flow rate of hydrogen chloride to 10~30Nm 3 / h, until the material in the kettle is completely dissolved and clarified, stop passing hydrogen chloride. Cool down to about 60°C, discharge the material to the rectification kettle (with stirring), add 720 kg of benzene, heat up and rectify, control the temperature at the top of the tower at 64~65°C, and extract 952.5 kg of distillate. After the tower top temperature was 68~69°C and there was no production, 15.6 kg of distillate was distil...

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PUM

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Abstract

The invention discloses an improved method for preparing glycine ethyl ester hydrochloride. The method includes the steps of putting glycine, ethyl alcohol and hydrogen chloride according to a certainratio for salinization and esterification, adding dehydrant for evaporating water, conducting cooling, crystallizing, centrifugal separating and drying to obtain a product, adding a certain volume ofwater to a three-element system composed of the evaporated dehydrant, ethyl alcohol and water for standing and phase separating, directly recycling a phase layer of the dehydrant, conducting phase separating to obtain a water phase for recovering ethyl alcohol for use, and recycling a centrifugal mother solution for material putting. After salinization and esterification of glycine, the content of water in esterification liquid is reduced, glycine hydrochloride can continue to be esterified into glycine ethyl hydrochloride in the rectification process, the generated water is taken away at thesame time, and the product conversion rate is increased; the mother solution obtained after crystallization and centrifugation is recycled without distillation, neutralization and rectification treatment of each batch, the treatment amount of leftovers and waste salt is reduced, and energy consumption is also reduced. Meanwhile, the content of glycine hydrochloride is reduced, so the product quality is improved.

Description

technical field [0001] The invention relates to a method for preparing glycine ethyl ester hydrochloride. Background technique [0002] The chemical name of glycine ethyl ester hydrochloride is ethyl glycine hydrochloride, a widely used pesticide and pharmaceutical intermediate, and can also be used in biochemical research and as a feed additive. In the synthesis of pesticides, ethyl glycinate hydrochloride is a key intermediate of various pyrethroid pesticides such as permethrin, allethrin, resmethrin, tetramethrin, and metethrin. Pyrethroid insecticides are currently the most widely used class of insecticides in the world, and are widely used in agriculture, storage and life hygiene and other fields. It can also be used to synthesize pesticides such as iprodione. In medicine synthesis, it can be used to synthesize anti-inflammatory drugs such as gemifloxacin, such as Chinese patent CN104725294A, which uses ethyl glycine hydrochloride and 4-halogenated acetoacetate as raw...

Claims

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Application Information

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IPC IPC(8): C07C227/18C07C229/08
CPCC07C227/18C07C229/08
Inventor 张继钱江飞李红梅施云云
Owner 江苏优普生物化学科技股份有限公司
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