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Synthetic method for 4-amino-3-phenylbutyric acid hydrochloride

A technology of phenylbutyrate hydrochloride and synthesis method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., and can solve problems such as high price of starting materials, heavy pollution in the production process, and cumbersome operation steps , to achieve the effect of low cost, high yield and simple process

Inactive Publication Date: 2015-04-01
SHAANXI JIAHE PHYTOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention provides a method for synthesizing 4-amino-3-phenylbutyrate hydrochloride, which mainly solves the problems of high price of starting raw materials used in the existing technology, complicated operation steps and large pollution in the production process

Method used

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  • Synthetic method for 4-amino-3-phenylbutyric acid hydrochloride
  • Synthetic method for 4-amino-3-phenylbutyric acid hydrochloride
  • Synthetic method for 4-amino-3-phenylbutyric acid hydrochloride

Examples

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Effect test

example 1

[0026] 1] Preparation of the first intermediate:

[0027] Add 265g (2.5mol) of benzaldehyde, 812.5g (6.25mol) of ethyl acetoacetate, and 20g of piperazine into 1000ml (97%) of ethanol, stir and react for 48 hours at room temperature 20°C-25°C, filter, rinse with absolute ethanol The filter cake was dried to obtain 700 g of solid, and the filtrate was concentrated to 1 / 4 of the original volume, cooled, filtered and washed with alcohol to obtain another 50 g of solid, which was combined twice for a total of 750 g, with a yield of 78%;

[0028] 2] Preparation of the second intermediate:

[0029] Add 280g (0.11mol) of the intermediate to 400mL of 20% sodium hydroxide solution (80g of sodium hydroxide dissolved in 320mL of water), stir at 85-90°C for 2-2.5h, filter, wash the filter cake with water, and combine Filtrate, cooling the filtrate, adding 170 mL of hydrochloric acid dropwise under stirring and cooling to adjust the pH to 1-2, stirring under cooling for 3 h, filtering, wa...

example 2

[0037] 1] Preparation of the first intermediate:

[0038] Add 53g (0.5mol) of benzaldehyde, 162.5g (1.25mol) of ethyl acetoacetate, and 25g of triethylamine into 200ml of 95% (97%) ethanol, stir and react for 48h at room temperature at 20°C-25°C, filter, and wash with absolute ethanol Rinse the filter cake and dry to obtain 140 g of solid, concentrate the filtrate to 1 / 4, cold analyze, filter and wash with alcohol to obtain 6 g of solid, and combine the two solids to obtain 146 g in total, with a yield of 83%;

[0039] 2] Preparation of the second intermediate:

[0040] Add 140g (0.11mol) of the intermediate to 400mL of 20% sodium hydroxide solution (80g sodium hydroxide dissolved in 320mL water), stir and react at 85-90°C for 2-2.5h, filter, wash the filter cake with water, combine the filtrates, and cool To the filtrate, 170 mL of HCl was added dropwise with stirring and cooling to adjust the pH to 1-2, and the mixture was stirred for 3 h under cooling, filtered, washed wit...

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Abstract

The invention provides a synthetic method for 4-amino-3-phenylbutyric acid hydrochloride. The synthetic method for 4-amino-3-phenylbutyric acid hydrochloride prepares 4-amino-3-phenylbutyric acid hydrochloride by preparing a first intermediate, a second intermediate, a third intermediate, preparing 4-amino-3-phenylbutyric acid and forming a salt. The synthetic method is a complete technology for synthesizing 4-amino-3-phenylbutyric acid hydrochloride, is simple in technology, high in yield and relatively low in cost, and mainly solves the problems that initial raw materials employed in the prior art are high in price, operation steps are tedious and the production process has large pollution.

Description

technical field [0001] The invention relates to a method for synthesizing 4-amino-3-phenylbutyrate hydrochloride. Background technique [0002] The structural formula of 4-amino-3-phenylbutyrate hydrochloride is as follows: [0003] [0004] At present, the synthetic method of the disclosed 3-benzyloxy-butylaniline hydrochloride is as follows: using m-aminophenol as a raw material, undergoing butyrylation and Fries rearrangement to obtain 2-butyryl-5-butyramide Base phenol: Under the action of alkali, 2-butyryl-5-butyrylamide phenol reacts with benzyl halide to generate 2-butyryl-5-butyrylamide phenylbenzyl ether, which is then hydrolyzed to obtain 3-benzyloxy- 4-Butyrylaniline, finally through the reduction reaction of Huang Minglong, was formed into a salt to obtain 3-benzyloxy-4-butylaniline hydrochloride. The price of starting raw materials used in the above process is high, the operation steps are complicated, and the production process pollutes a lot. Contents o...

Claims

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Application Information

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IPC IPC(8): C07C227/04C07C229/34
Inventor 郭文华肖金霞惠战锋徐亦为
Owner SHAANXI JIAHE PHYTOCHEM
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