Preparation method of high-activity palladium-carbon catalyst for synthesis of imipenem antibiotics

The technology of a palladium-carbon catalyst and an antibiotic is applied in the field of preparation of a high-activity palladium-carbon catalyst, which can solve the problems of low catalyst activity and selectivity, poor filterability and the like, and achieve the effects of improving the effective utilization rate and high activity.

Inactive Publication Date: 2013-04-17
SINO PLATINUM METALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The purpose of the present invention is to overcome the deficiencies of the above-mentioned prior art, especially for the shortcomings of existing catalysts with low activity and selectivity and poor filterability, and provide a method for preparing a high-efficiency palladium-carbon catalyst for the synthesis of penem antibiotics

Method used

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  • Preparation method of high-activity palladium-carbon catalyst for synthesis of imipenem antibiotics
  • Preparation method of high-activity palladium-carbon catalyst for synthesis of imipenem antibiotics
  • Preparation method of high-activity palladium-carbon catalyst for synthesis of imipenem antibiotics

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preparation example Construction

[0035] The preparation method of the palladium-carbon catalyst used for the synthesis of penem antibiotics of the present invention uses chloropalladium acid and its salt as the precursor compound of the active component palladium, takes powdered activated carbon as the carrier, and adds sodium citrate or sodium citrate in the Pd impregnation solution Sodium acetate, then the Pd impregnation solution is adsorbed on the active carbon in sections, and obtains the palladium carbon catalyst through wet chemical reduction, and the concrete steps are as follows:

[0036] (1) In the mixed slurry of activated carbon and ionized water, pre-adsorb sodium citrate or sodium acetate complexing agent;

[0037] (2) prepare palladium salt solution, add dropwise in the slurry that step (1) obtains, palladium load is 5%~10%;

[0038] (3) Sectional adsorption of palladium salt solution, the pH of the first step is controlled between 4 and 5, and the pH of the second step is controlled between 9 ...

Embodiment 1

[0050] Example 1: 1) Weigh 180 g (dry weight) of activated carbon, add it to a 5 L reactor, add 0.9 L of water, and stir for 2 h;

[0051] 2) Weigh 33.2 g PdCl 2 , add 20 ml of concentrated hydrochloric acid and 1 L of deionized water, heat to boiling to dissolve, and cool to room temperature;

[0052] 3) Add the palladium salt solution obtained in step) 2 to the activated carbon slurry at a constant speed. After dropping, adjust the pH of the slurry to 4.5 with 10% NaOH, stir and adsorb for 5 h, and then add 10% NaOH dropwise to adjust the pH value , keep the pH value between 9-10, and stir the deposition to continue to adsorb for 16 h;

[0053] 4) At 80 °C, add 70 ml of formaldehyde, keep the pH at 9-10, and reduce for 4 h;

[0054] 5) Cool, let it stand overnight, filter, wash with deionization until the filtrate is neutral, and obtain a 10% Pd / C catalyst with a water content of 58.6%.

Embodiment 2

[0055] Example 2: 1) Weigh 180 g (dry weight) of activated carbon and 13.5 g of sodium citrate into a 5 L reactor, add 0.9 L of water, and stir for 2 h;

[0056] 2) Weigh 33.2 gPdCl 2 , add 20 ml of concentrated hydrochloric acid and 1 L of deionized water, heat until boiling and dissolve, add 20 g of sodium citrate, and heat for another 10 minutes, without bumping the solution, then cool to room temperature;

[0057] 3) Add the palladium salt solution obtained in step 2) into the activated carbon slurry at a constant speed. After dropping, use the slurry to have a pH of 4.6, stir and adsorb for 5 hours, then add 10% NaOH dropwise to adjust the pH value, and keep the pH value at 9 Between -10, the stirring deposition continued to adsorb for 16 h;

[0058] 4) At 80 °C, add 70 ml of formaldehyde, keep the pH at 9-10, and reduce the time for 4 h;

[0059] 5) Cool, let it stand overnight, filter, wash with deionization until the filtrate is neutral, and obtain a 10% Pd / C catalys...

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Abstract

The invention relates to a preparation method of a high-activity palladium-carbon catalyst for synthesis of imipenem antibiotics. According to the preparation method of the high-activity palladium-carbon catalyst for the synthesis of the imipenem antibiotics, ammonium chloropalladite and salts thereof are taken as precursor compounds of an active component, namely palladium, powdered activated carbon is taken as a carrier, additives such as sodium citrate are added into Pd impregnation liquid, and then the Pd impregnation liquid is absorbed onto the activated carbon in a segmenting manner and subjected to wet chemical reduction to obtain the high-activity palladium-carbon catalyst; and the catalyst is used for industrial production of the synthesis of the imipenem antibiotics.

Description

technical field [0001] The invention relates to a preparation method of a high-activity palladium-carbon catalyst, in particular to a preparation method of a high-activity palladium-carbon catalyst for removing benzylic protecting groups in the synthesis of penem drugs. Background technique [0002] Benzyl is an important protective group for organic functional groups. Because it is easy to form, relatively stable under certain conditions and easy to remove under mild conditions, it is often used to protect compounds containing O- and N- in organic synthesis. After protection, the corresponding benzyl ether, benzyl ester and benzylamine were prepared respectively. In the process of debenzylation, the benzyl group is separated from the amino or hydroxyl functional group, and the benzyl or substituted benzyl group is hydrogenolyzed to form toluene or substituted toluene and removed, and the compound itself generally does not cause damage. An attractive use of debenzylation (o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J35/10C07D477/20C07D477/08
Inventor 戴云生唐春潘再富沈亚峰左川冯洋洋
Owner SINO PLATINUM METALS CO LTD
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