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Palladium tin carbon catalyst for meropenem synthesis and preparation method

A technology of carbon catalyst and meropenem, which is applied in the direction of chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc. Activity is not easy to control and other problems, to achieve the effect of inhibiting migration growth, maintaining stability, and improving utilization

Inactive Publication Date: 2011-07-27
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Catalysts prepared by this type of process, for catalyst producers, have the disadvantages of complex and lengthy process preparation, difficult control of activity, and high possibility of excessive poisoning, and cannot reduce the cost of use for catalyst users

Method used

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  • Palladium tin carbon catalyst for meropenem synthesis and preparation method
  • Palladium tin carbon catalyst for meropenem synthesis and preparation method
  • Palladium tin carbon catalyst for meropenem synthesis and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1 (5% Pd / C)

[0031] 1) Accurately weigh 19g of coconut shell charcoal with a particle size of 200-300 mesh. Reflux with 8% boiling phosphoric acid aqueous solution for 2 hours, wash with pure water to pH = 6, then treat with 8% sodium hypochlorite aqueous solution at 30-35°C for 2 hours, and finally wash with pure water until silver nitrate detects that there is no chlorine ion for later use ;

[0032] 2) Accurately weigh 3.13g of potassium chloropalladate, dissolve it in pure water, dilute to 60mL in an ice bath and cool down to 0-5°C, weigh 0.16g of stannous chloride, dissolve in 0.5mL of concentrated hydrochloric acid and dilute to 60mL in an ice bath Cool down to 0-5°C, and quickly pour the stannous chloride solution into the palladium acid solution under stirring conditions;

[0033] 3) 19g of weighed activated carbon is beaten with 300mL of 10% sodium carbonate solution, heated to 55-60°C under stirring conditions and stabilized for 1h;

[0034] 4) Pou...

Embodiment 2

[0036] Example 2 (5% Pd / C)

[0037] 1) Accurately weigh 19g of coconut shell charcoal with a particle size of 200-300 mesh, reflux treatment with 8% boiling phosphoric acid aqueous solution for 2h, wash with pure water to pH=6, and then use 8% sodium hypochlorite aqueous solution at 30-35°C Treat for 2 hours, and finally wash with pure water until there is no chloride ion detected by silver nitrate for later use;

[0038] 2) Accurately weigh 3.13g of potassium chloropalladate, dissolve it in pure water, dilute to 60mL in an ice bath and cool down to 0-5°C, weigh 0.16g of stannous chloride, dissolve in 0.5mL of concentrated hydrochloric acid and dilute to 60mL in an ice bath Cool down to 0-5°C, and quickly pour the stannous chloride solution into the palladium acid solution under stirring conditions;

[0039] 3) 19g of weighed activated carbon is beaten with 300mL of 10% sodium carbonate solution, heated to 55-60°C under stirring conditions and stabilized for 1h;

[0040] 4) Po...

Embodiment 3

[0042] Embodiment 3 (5%Pd / C)

[0043] 1) Accurately weigh 19g of coconut shell charcoal with a particle size of 200-300 mesh. Reflux with 8% boiling phosphoric acid aqueous solution for 2 hours, wash with pure water to pH = 6, then treat with 8% sodium hypochlorite aqueous solution at 30-35°C for 2 hours, and finally wash with pure water until silver nitrate detects that there is no chlorine ion for later use ;

[0044] 2) Accurately weigh 3.13g of potassium chloropalladate, dissolve it in pure water, dilute to 60mL in an ice bath and cool down to 0-5°C, weigh 0.16g of stannous chloride, dissolve in 0.5mL of concentrated hydrochloric acid and dilute to 60mL in an ice bath Cool down to 0-5°C, and quickly pour the stannous chloride solution into the palladium acid solution under stirring conditions;

[0045] 3) 19g of weighed activated carbon is beaten with 300mL of 10% sodium carbonate solution, heated to 55-60°C under stirring conditions and stabilized for 1h;

[0046] 4) P...

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Abstract

The invention discloses a palladium carbon catalyst for meropenem synthesis and a preparation method. In the catalyst, powdery active carbon is used as a carrier and loads active ingredient Pd metal and active ingredient Sn. The preparation method comprises the following steps of: after the active carbon carrier is sequentially treated by using inorganic acid and sodium hypochlorite, washing the active carbon carrier to be neutral for later use by using pure water; preparing active ingredient solution by using water-soluble Pd containing compound and diluted hydrochloric acid solution of stannous chloride in a ratio; pulping the active carbon of metered weight by using aqueous solution of alkali compound with certain concentration, heating the pulp to the temperature of between 40 and 65 DEG C with stirring and stabilizing the pulp for 1 hour; and guiding the mixed solution of Pd and Sn in a metering ratio into the active carbon pulp, continually stirring the solution for 3 to 6 hours to load the Pd and the Sn on the active carbon to obtain a catalyst precursor, ageing the catalyst precursor, and reducing the catalyst precursor by using a reducing agent to obtain a catalyst product. The palladium carbon noble metal content can be reduced to below 5 percent from 10 percent, the yield of the product is improved by 3 to 4 percent, and the using cost is effectively reduced when the yield of the product is improved.

Description

technical field [0001] The invention belongs to the technical field of medicine preparation, and relates to a supported palladium-carbon catalyst for catalyzing hydrogenolysis reaction, in particular to a palladium-tin-carbon catalyst for synthesizing meropenem and a preparation method thereof. Background technique [0002] Half a century after Alexander Fleming invented penicillin, a new member of antibiotics - carbapenem antibiotics (hereinafter referred to as "penem") was born. Penem has a wide range of antibacterial properties and strong antibacterial activity. It has played an extremely important role in the control of drug-resistant bacteria, enzyme-producing bacteria infections, and immunodeficiency infections. Its excellent clinical efficacy against methicillin-resistant Staphylococcus aureus has received attention. Although the production of such antibiotics is relatively difficult and the production process is relatively complicated, they are the most resistant an...

Claims

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Application Information

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IPC IPC(8): B01J23/62C07D477/20C07D477/06
Inventor 李岳峰张之翔曾永康曾利辉谭小艳杨乔森
Owner XIAN CATALYST NEW MATERIALS CO LTD
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