A kind of preparation method of 4-amino-cyclohexylacetic acid

A technology of nitrophenylacetic acid and amino, which is applied in the preparation of organic compounds, cyanide reaction preparation, chemical instruments and methods, etc., to achieve the effect of simple collection operation, low price, and favorable large-scale industrial production

Active Publication Date: 2018-04-06
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method of preparing high value-added chemicals by catalytic hydrogenation of 4-nitrophenylacetic acid has not been well perfected. It is important to explore efficient and simple hydrogenation methods to convert 4-nitrophenylacetic acid into more valuable chemicals. much needed

Method used

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  • A kind of preparation method of 4-amino-cyclohexylacetic acid
  • A kind of preparation method of 4-amino-cyclohexylacetic acid
  • A kind of preparation method of 4-amino-cyclohexylacetic acid

Examples

Experimental program
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Effect test

preparation Embodiment 1

[0025] Preparation Example 1: Preparation of 3%Pd-5%Ni / C catalyst by deposition precipitation method

[0026] Take by weighing 155g palladium chloride (the content of metal palladium is 59.5wt%), 740g nickel nitrate hexahydrate adds 30kg deionized water, adds 2.760kg carrier gac, fully stirs, with the sodium hydroxide solution of 0.5wt% the previous step Adjust the pH of the slurry to about 7, and stir at room temperature for 18 hours. After the reaction, filter and wash the slurry until the filtrate becomes neutral and free of chloride ions. Add 20 kg of deionized water to the washed filter cake, add 1.5 L of formaldehyde, and set the temperature at 50 ° C. After reacting for 2 hours, the active component metal is reduced to obtain a 3%Pd-5%Ni / C catalyst.

preparation Embodiment 2

[0027]Preparation Example 2: Preparation of 3%Pd-3%Ru / C catalyst by deposition precipitation method

[0028] Take by weighing 155g palladium chloride (the content of metal palladium is 59.5wt%) and 250g ruthenium chloride (the content of metal ruthenium is 37.5wt%), add 30kg deionized water after dissolving with 2L 15wt% sodium chloride solution, add 3kg carrier activated carbon, fully stirred, adjust the pH of the slurry in the previous step to about 8 with 10wt% sodium bicarbonate solution, stir in a water bath at 30°C for 1 hour, after the reaction, filter and wash the slurry until the filtrate is neutral and chlorine-free ions, add 20kg of deionized water to the washed filter cake, add 2.5L of formaldehyde, react at 50°C for 1h, and reduce the active component metal palladium to obtain a 3%Pd-3%Ru / C catalyst.

preparation Embodiment 3

[0029] Preparation Example 3: Preparation of 2%Au-3%Pd / C Catalyst by Deposition and Precipitation Method

[0030] Take by weighing 90g gold chloride (the content of metal gold is 47.8wt%), 155g palladium chloride (the content of metal palladium is 59.5wt%), add after dissolving with 1000kg deionized water, add 1.9kg carrier gac, fully stir, Use 10wt% sodium bicarbonate solution to adjust the pH of the slurry in the previous step to about 7, stir in a water bath at 80°C for 2h, filter, wash until there are no chloride ions, dry, and reduce with hydrogen, and reduce at 300°C for 3h to obtain 2%Au-3%Pd / C catalyst.

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Abstract

The invention discloses a 4-nitrophenylacetic-acid-catalyzing hydrogenation preparing method for trans-4-amino-cyclohexylacetic acid and hydrochloride. Under the condition of a multiple-active-component supported catalyst prepared with the method, a hydrogenation reaction has the high activity and selectivity, operating is easy, the cost of the catalyst is low, and other reaction steps are not required; the technology is 4-nitrophenylacetic-acid heterogeneous catalysis and hydrogenation, the reaction condition is mild, the method is efficient, simple, easy to carry out, economical and free of pollution, the technology is simple, and large-scale industrial production is facilitated.

Description

technical field [0001] The invention relates to a method for preparing trans-4-amino-cyclohexylacetic acid and hydrochloride by catalyzing the hydrogenation of 4-nitrophenylacetic acid, in particular to the preparation of selective hydrogenation of 4-nitrophenylacetic acid catalyzed by multi-active component catalysts Trans-4-amino-cyclohexaneacetic acid and hydrochloride. Background technique [0002] 4-Aminophenylacetic acid, phenylacetic acid, cyclohexaneacetic acid, cis-4-amino-cyclohexylacetic acid, and trans-4-amino-cyclohexylacetic acid are very important chemical raw materials, widely used in the synthesis of new materials and pharmaceutical research and development and other important areas. Among them, trans-4-amino-cyclohexylacetic acid is widely used in medicine and is a very important intermediate for the synthesis of drugs. The way of hydrogenation of 4-nitrophenylacetic acid to produce high value-added chemicals is as follows: [0003] [0004] In the pa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/48C07C227/04C07C227/18B01J27/20
CPCB01J27/20C07C227/04C07C227/18C07C229/48
Inventor 牟新东王喜成李慧
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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