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Synthesis method of beta-alanine methyl ester salt product

A kind of technology of alanine methyl ester and synthesis method, which is applied in the field of synthesis of β-alanine methyl ester salt products, can solve the problems of a large number of organic solvents, toxicity, harsh production environment requirements, etc., and achieve low environmental pollution and easy control , the effect of simple operation

Inactive Publication Date: 2017-01-11
JING JING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the synthesis method of β-alanine methyl ester salt has complex conditions, requires a large amount of organic solvents, and has extremely harsh requirements on the production environment.
At the same time, the industrially synthesized β-alanine methyl ester salt is mainly β-alanine methyl ester hydrochloride (chemical formula is C 4 h 9 NO 2 HCl), its molecule contains hydrogen chloride, which has certain toxicity and is not conducive to large-scale safe production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 300g of β-alanine and add it into 1900g of methanol and stir, and slowly add 400g of concentrated sulfuric acid at 19-21°C. After the addition of concentrated sulfuric acid, the temperature was raised to 65-68°C, refluxed for 8 hours, and the temperature was lowered to 24°C. The methanol solution of β-alanine methyl ester sulfate was concentrated under vacuum at 45°C until no methanol was evaporated. The concentrated solution was lowered to 22°C, 2500ml of purified water was added, and the pH of the β-alanine methyl sulfate aqueous solution was adjusted to 2.5 with ammonia water. Store the prepared β-alanine methyl ester sulfate aqueous solution at 7°C.

[0022] Obtain 2850ml of β-alanine methyl ester sulfate aqueous solution, the content of methyl ester is 115.7g / L, and the yield of methyl ester is 95%.

Embodiment 2

[0024] Take 300g of β-alanine and add it into 1900g of methanol and stir, and slowly add 400g of concentrated sulfuric acid at 19-21°C. After the addition of concentrated sulfuric acid, the temperature was raised to 65-68°C, refluxed for 8 hours, and the temperature was lowered to 23°C. The methanol solution of β-alanine methyl ester sulfate was concentrated under vacuum at 45°C until no methanol was evaporated. The concentrated solution was lowered to 23°C, 2500ml of purified water was added, and the pH of the β-alanine methyl sulfate aqueous solution was adjusted to 2.5 with ammonia water. Store the prepared β-alanine methyl ester sulfate aqueous solution at 7°C.

[0025] Obtain 2850ml of β-alanine methyl ester sulfate aqueous solution, the content of methyl ester is 112g / L, and the yield of methyl ester is 92%.

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Abstract

The invention discloses a synthesis method of a beta-alanine methyl ester salt product, and relates to the technical field of beta-alanine methyl ester salt production. The method includes the following steps of firstly, adding beta-alanine to methyl alcohol to be stirred, and adding concentrated sulfuric acid; secondly, conducting backflow after feeding of concentrated sulfuric acid ends; thirdly, concentrating a methyl alcohol solution of beta-alanine methyl ester salt; fourthly, adding the concentrated solution to purified water to be evenly stirred, adjusting the PH of a water solution of beta-alanine methyl ester salt through ammonium hydroxide, and storing the prepared water solution of beta-alanine methyl ester salt at low temperature. The method has the advantages of being high in yield, easy to operate and easy to control; the method is free of toxic and corrosive gases in the synthesis process, small in environment pollution and beneficial to large-scale production.

Description

technical field [0001] The invention relates to the technical field of production methods of β-alanine methyl ester salt products. Background technique [0002] Alanine methyl ester salt is mainly used as pharmaceutical intermediates and scientific research reagents, and is widely used in scientific research such as molecular biology and pharmacology. [0003] β-alanine methyl ester salt is very soluble in water, ethanol, acetone and other organic solvents. At present, the synthesis method of β-alanine methyl ester salt has complex conditions, requires a large amount of organic solvents, and has extremely strict requirements on the production environment. At the same time, the industrially synthesized β-alanine methyl ester salt is mainly β-alanine methyl ester hydrochloride (chemical formula is C 4 h 9 NO 2 ·HCl), its molecules contain hydrogen chloride, which has certain toxicity and is not conducive to large-scale safe production. Contents of the invention [0004]...

Claims

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Application Information

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IPC IPC(8): C07C227/18C07C229/08
CPCC07C227/18C07C229/08
Inventor 李斌水米造吉刘玉兵马静杨涛
Owner JING JING PHARMA
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