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 prepar...

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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