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Method of preparing 4-amino-3-phenyl butyric hydrochloride

A technology of phenylbutyric acid hydrochloride and amino, which is applied in the preparation of organic compounds, chemical instruments and methods, and preparation of cyanide reactions, etc. It can solve the problems of complicated operation steps, high price of starting materials, and large pollution in the production process. problems, to achieve the effect of simple production process, low price and high product yield

Inactive Publication Date: 2007-09-12
安徽省郎溪县科联实业有限公司 +1
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AI Technical Summary

Problems solved by technology

The starting raw materials used in the above process are expensive, the operation steps are cumbersome, and the production process is polluted.

Method used

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Embodiment Construction

[0013] Put in benzoic acid, methanol and nitromethane in a weight ratio of 1:8:0.5, keep warm at 18°C ​​for 10 hours, cool and crystallize to 5°C, then separate solid and liquid, and dry to obtain nitrostyrene.

[0014] The dried nitrostyrene and diethyl malonate are put into methanol solution, and the nitrostyrene, diethyl malonate and methanol solution are configured in a weight ratio of 1:1.40:5. Then, heat up to 45°C for 2 hours, stir and react to generate α-methoxymethyl-β-phenyl-г-nitrobutyric acid methyl ester, then drop into Ni respectively by 10% and 2.5% of the weight of nitrostyrene and H 2 . Then, keep the temperature at 50° C. and the pressure at 4 MPa to carry out hydrogenation reaction for 12 hours to obtain α-carbomethoxy-β-phenyl-г-tetrahydropyrrolidone.

[0015] Raise the temperature of a-methoxy-β-phenyl-г-tetrahydropyrrolidone to 80°C, drop in twice the amount of hydrochloric acid of a-carbomethoxy-β-phenyl-г-tetrahydropyrrolidone for hydrolysis, and the ...

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PUM

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Abstract

This invention relates to a preparation method for 4-amido-phenyl butyrate including: mixing benzene formate and methyl alcohol with nitromethane to be reacted at heat preservation, cooled and crystallized, separated for solid and liquid to be dried to get nitrobenzene ethane, which is put into a methanol solution together with diethyl malonate to be reacted to generate alpha-carbomethoxy-beta-phenyl-gamma-nitryl methyl butyrate, then Ni and H2 are added into a methanol solution to carry out hydrogenation reaction to get alpha-carbomethoxy-beta-phenyl-gamma tetrahydroketopyrrolidine, which is added with HCl to be hydrolyzed dried to get a product of 4-amido-phenyl butyrate.

Description

technical field [0001] The invention relates to a method for preparing chemical products, namely a new method for preparing 4-amino-3-phenylbutyrate hydrochloride. Background technique [0002] At present, the preparation method of 3-benzyloxy-4-butylaniline hydrochloride in China is as follows: using m-aminophenol as raw material, undergoing butylation reaction and Fries rearrangement to obtain 2-butyryl-5-buty Aminophenol; under the action of alkali, 2-butyryl-5-butyrylaminophenol reacts with benzyl halide to generate 2-butyryl-5-butyrylamidophenylbenzyl ether, which is then hydrolyzed to obtain 3-benzyloxy -4-butyrylaniline, and finally through the reduction reaction of Huang Minglong, the salt was formed 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 the invention [0003] The technical problem to be s...

Claims

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Application Information

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IPC IPC(8): C07C229/08C07C227/22
Inventor 刘种权
Owner 安徽省郎溪县科联实业有限公司
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