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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

Active Publication Date: 2015-03-11
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

[0028] 1] Add 250kg of water into a 1000L reactor, and control the temperature in an ice bath below 15°C, then add 70kg of ethyl acetoacetate into the reactor, stir vigorously and control the temperature not to exceed 15°C; while stirring, dropwise add a mass concentration of 40% sodium hydroxide solution and 70kg mass concentration 99% benzoyl chloride solution keep the pH of the reaction system at about 10. After the dropwise addition, let stand at 55°C for 4-5h; then lower the temperature to 25°C, add 100kg of saturated saline, stir slowly for 10-30 hours, then carry out liquid separation treatment, wash the oily matter with water, and dry over anhydrous sodium sulfate , That is ethyl benzoylacetate.

[0029] 2.1] Get nitromethane 62kg and benzaldehyde 110kg methyl alcohol 400kg and join in the 1000L reactor of step 1 and cool to 0 ℃, then add the sodium hydroxide solution 200kg of concentration 40%, react for three hours after adding, add water and The mass concentration ...

example 2

[0036] 1] Add 500kg of water to a 2000L reactor and control the temperature in an ice bath below 15°C, add 140kg of ethyl acetoacetate, stir vigorously, add dropwise sodium hydroxide with a mass concentration of 40%, control the temperature not exceeding 15°C, and start simultaneously 140 kg of benzoyl chloride with a mass concentration of 99% was added dropwise to control the rate of addition of the two, so that the pH of the reaction system was maintained at about 10, and the reaction system was left to stand at 55° C. for 4-5 hours after the drop was completed. Then, at 25°C, 200 kg of saturated saline was added, slowly stirred overnight, reacted for 20 hours, separated, the oil was washed with water, and dried over anhydrous sodium sulfate. That is ethyl benzoyl acetate.

[0037] 2.1] nitromethane 124kg and benzaldehyde 220kg methanol 800kg join in 2000L reaction kettle and cool down to 0 degree, add mass concentration and be 40% sodium hydroxide 200kg, react for three hou...

example 3

[0044]1] Add 750kg of water to the 3000L reactor and control the temperature in an ice bath below 15°C, add 210kg of ethyl acetoacetate, stir vigorously, add dropwise sodium hydroxide with a mass concentration of 40%, control the temperature not to exceed 15°C, and start simultaneously Add 210 kg of benzoyl chloride with a mass concentration of 99% dropwise to control the drop rate of the two, so that the pH of the reaction system is maintained at about 10. Ethyl acetate, after the drop is completed, let stand at 55°C for 4-5h. Then, at 25°C, 300 kg of saturated saline was added, slowly stirred overnight, reacted for 20 hours, separated, the oil was washed with water, and dried over anhydrous sodium sulfate. That is ethyl benzoyl acetate.

[0045] 2.1] Nitromethane 186kg and benzaldehyde 360kg methyl alcohol 1200kg join in 3000L reactor and cool to 0 degree, add mass concentration and be 40% sodium hydroxide 200kg, react for three hours after adding, add water 300kg, add conce...

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Abstract

A provided synthetic method for 4-amino-3-phenylbutyric acid hydrochloride comprises the steps: preparing ethyl benzoylacetate, preparing nitroethenylbenzene, preparing an addition product, and processing to obtain the product. The synthetic method is an integral technology for synthesizing 4-amino-3-phenylbutyric acid hydrochloride. The method is simple in technology, high in yield and relatively low in cost, and mainly solves the problems that an initial raw material used in the prior art is high in price, operation steps are tedious and a production process is large in pollution.

Description

technical field [0001] The invention relates to a synthesis method of 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 of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/34C07C227/04
Inventor 郭文华肖金霞肖红王晓莹邓尚勇
Owner SHAANXI JIAHE PHYTOCHEM
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