Method for preparing betaine hydrochloride

A technology of betaine hydrochloride and dilute hydrochloric acid, applied in chemical instruments and methods, cyanide reaction preparation, preparation of organic compounds, etc., can solve the problems of easy existence of safety, high cost, strong irritation, etc., and achieve mild reaction conditions. , safety assurance, cost reduction effect

Active Publication Date: 2011-12-07
杭州海尔希畜牧科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are three main preparation methods of betaine, one is prepared by reacting glycine and diazomethane (Chemische Berichte, 83, 420-431, 1950), However, since diazomethane is a gas at room temperature, and is explosive, flammable, highly toxic and highly irritating, special conditions are required for transportation, storage and use, and there are likely to be potential safety hazards
The second method is prepared by reacting trimethylamine and chloroacetic acid (US 5696287). This method is a production me

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A method for preparing betaine hydrochloride, the steps are:

[0031] a. Add 1mol ethyl chloroacetate 122.5g and ethanol 500g in the 1500ml three-neck bottle that reflux condenser, thermometer, air guide tube, tail gas absorption device and magnetic stirring device are housed, be placed on the ice-water bath under stirring, make reaction mixture cool down to Below 10°C;

[0032] b. Pass 59 g of 1 mol of anhydrous trimethylamine gas into the mixture, keep the reaction temperature not exceeding 20°C during the gas flow, continue to stir for 1 hour after passing through, collect the solid product by filtration, and recrystallize through acetonitrile at 90°C / 10mmHg Drying at low temperature for 6 hours gave 173.7 g of 2-ethoxy-2-oxa-N,N,N-trimethyl-ethylammonium chloride, melting point 151-153°C, yield 95.7%;

[0033] c. In a 2000ml three-necked flask equipped with a reflux condenser, a thermometer and a magnetic stirring device, add 181.5g of 1mol of 2-ethoxy-2-oxa-N,N...

Embodiment 2

[0037] A method for preparing betaine hydrochloride, the steps are:

[0038] a. Add 1mol ethyl chloroacetate 122.5g and ethanol 980g in the 1500ml three-neck flask that reflux condenser, thermometer, air guide tube, tail gas absorbing device and magnetic stirring device are housed, be placed on ice-water bath under stirring, make reaction mixture cool down to Below 10°C;

[0039] b. Pass 65g of 1.1mol anhydrous trimethylamine gas into the mixture, keep the reaction temperature not exceeding 20°C during the gas pass-in process, continue to stir for 2 hours after the pass-in is complete, filter and collect the solid product, and recrystallize through acetonitrile at 90°C / Dry at 10 mmHg for 6 hours to obtain 175.5 g of 2-ethoxy-2-oxa-N,N,N-trimethyl-ethylammonium chloride with a melting point of 151-153°C and a yield of 96.7%;

[0040]c. In a 2000ml three-necked flask equipped with a reflux condenser, a thermometer and a magnetic stirring device, add 181.5g of 1mol of 2-etho...

Embodiment 3

[0044] A method for preparing betaine hydrochloride, the steps are:

[0045] a. Add 1mol ethyl chloroacetate 122.5g and isopropanol 370g in the 1500ml three-necked bottle that is equipped with reflux condenser, thermometer, air guide tube, tail gas absorbing device and magnetic stirring device, place on ice-water bath under stirring, make reaction mixture Cool down to below 10°C;

[0046] b. Pass 65g of 1.1mol anhydrous trimethylamine gas into the mixture, keep the reaction temperature not exceeding 20°C during the gas pass-in process, continue to stir for 2 hours after the pass-in is complete, filter and collect the solid product, and recrystallize through acetonitrile at 90°C / Dry at 10mmHg for 6 hours to obtain 162.3g of 2-ethoxy-2-oxa-N,N,N-trimethyl-ethylammonium chloride with a melting point of 151-153°C and a yield of 89.4%;

[0047] c. In a 2000ml three-necked flask equipped with a reflux condenser, a thermometer and a magnetic stirring device, add 181.5g of 1mol o...

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Abstract

The invention belongs to the technical field of feed additive and relates to a method for preparing betaine hydrochloride, which comprises the following steps: a, adding ethyl chloroacetate and methanol or isopropanol into the reactor, stirring uniformly and cooling the mixture; b, introducing trimethylamine anhydrous gas into the mixture, fully stirring after the trimethylamine anhydrous gas is introduced completely, filtering, recrystallizing collected solid product, drying under vacuum and obtaining 2-ethoxy-2-oxa-N,N,N-trimethyl-ethylammonium chloride; and c, adding 2-ethoxy-2-oxa-N,N,N-trimethyl-ethylammonium chloride and diluted hydrochloric acid into the reactor to obtain mixed solution, heating, reacting with stirring, distilling after reaction, filtering, drying collected solid product under vacuum, and thus, obtaining the refined betaine hydrochloride. In the invention, the reactions in the steps are normal operation, the safety of production is ensured, the need of using expensive raw material is obviated, the production cost is reduced, the final product does not contain sodium chloride, and the requirements of some special fields are met.

Description

technical field [0001] The invention belongs to the field of feed additives, in particular to a method for preparing betaine hydrochloride. Background technique [0002] In the development of the modern breeding industry, in order for the raised livestock and poultry to grow healthily during the growth period and have better quality after mature slaughter, in addition to the necessary staple food, some functional functions should be added during the feeding process. The auxiliary materials, that is, additives, these additives can effectively improve the quality of the cultured meat. [0003] In recent years, more and more attention has been paid to the application of betaine in the livestock and poultry industry. Because betaine can provide active methyl groups in the metabolism of biological organisms, form methyltransferases with cysteine, and participate in methylation reactions, so it is called "life methylating agent". [0004] At present, there are three main prepara...

Claims

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Application Information

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IPC IPC(8): C07C229/12C07C227/18
Inventor 楼伟杰谢创新
Owner 杭州海尔希畜牧科技有限公司
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