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Preparation method of platinum-carbon catalyst for efficient azithromycin synthesis

A platinum-carbon catalyst and azithromycin technology, applied in chemical instruments and methods, preparation of sugar derivatives, organic chemistry, etc., can solve the problems of activated carbon pore collapse, increase of platinum nanoparticles, and increase of platinum loss, and achieve uniform and rapid heating , convenient sampling and convenient maintenance

Inactive Publication Date: 2018-10-26
徐学军
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  • Abstract
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  • Claims
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Problems solved by technology

Although the patent CN 102652920 B mentions that the catalyst can be applied 4-8 times before processing, the 6,9-imino ether must be refined before it can be used, which increases the process and cannot avoid high-temperature acid-base treatment, while high-temperature acid Alkali treatment can easily lead to collapse of activated carbon pores, increased platinum loss, larger platinum nanoparticles, and irreversible decrease in activity
[0003] For this reason, we have conducted a detailed study on the reasons why commercially available platinum-carbon catalysts cannot be continuously used in the catalytic 6,9-imine ether hydrogenation reduction process. We found that the key factor causing catalyst deactivation is that the pores of activated carbon are used After being blocked, the active sites of the catalyst are partially covered and cannot be used again

Method used

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  • Preparation method of platinum-carbon catalyst for efficient azithromycin synthesis

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preparation example Construction

[0019] A kind of preparation method of efficient azithromycin synthetic platinum carbon catalyst of the present invention comprises the following steps:

[0020] a) Put the platinum precursor into water, stir and dissolve, add an organic acid to continue stirring and dissolving, the organic acid and the platinum precursor undergo a complexation reaction, and use an alkaline solution to adjust the pH of the solution;

[0021] b) gac is dropped into the solution of step a for impregnation;

[0022] c) After the impregnation is completed, transfer the solution in step b to the autoclave, first replace the air in the autoclave with nitrogen, then heat up the autoclave, then quickly pass hydrogen into the autoclave and keep it warm for 20 After ~1000 minutes, cool down and release the pressure;

[0023] d) After filtering and washing the solution in step c, the platinum carbon catalyst is obtained.

[0024] Specifically, the platinum precursor described in step a is a mixture of ...

Embodiment 1

[0031] In a 1000ml flask, add 300g of water and weigh 2.38g of H 2 PtC l6 ·6H 2 O was put into it and stirred to dissolve. Then add 2.36 grams of citric acid and continue stirring to dissolve. Raise the temperature to 40-45°C. Use 10% sodium hydroxide solution to adjust the pH between 5.5 and 5.6. Another 29.1 g of activated carbon was added. Keep warm overnight. Transfer to a high-pressure hydrogenation kettle, rapidly raise the temperature to 80° C., rapidly inject hydrogen gas to 3 MPa, and keep the temperature for 2 hours. After cooling, filtering and washing, 30 g of dry product equivalent of 3% Pt / C catalyst was obtained.

[0032] In a 1000ml flask, add 500 grams of methanol, cool to 5-10°C, add 100 grams of 6,9-imino ether, stir to dissolve, use hydrochloric acid (hydrochloric acid, citric acid, acetic acid, perchloric acid, hydrobromic acid can also be used) One or two or more of them are mixed) to adjust the pH to between 6.0 and 6.5. Transfer to an autoclave...

Embodiment 2

[0034] In a 1000ml flask, add 300g of water and weigh 3.98g of H 2 PtC l6 ·6H 2 O was put into it and stirred to dissolve. Then add 3.93 grams of citric acid and continue stirring to dissolve. Raise the temperature to 25-30°C. Use 10% sodium carbonate solution to adjust the pH between 5.5 and 5.6. Another 28.5 grams of activated charcoal was added. Keep warm overnight. Transfer to a high-pressure hydrogenation kettle, rapidly raise the temperature to 90° C., and rapidly pass hydrogen to 4 MPa, and keep the temperature for 2 hours. After cooling, filtering and washing, 30 g of dry product equivalent of 5% Pt / C catalyst was obtained.

[0035] In a 1000ml flask, add 500g of methanol, cool to 5-10°C, add 100g of 6,9-imide ether, stir to dissolve, use hydrochloric acid (hydrochloric acid, citric acid, acetic acid, perchloric acid, hydrobromic acid can also be used to One or two or more mixtures) to adjust the pH to between 6.0 and 6.5. Transfer to an autoclave and add the ...

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Abstract

The invention discloses a preparation method of a platinum-carbon catalyst for efficient azithromycin synthesis. The method comprises the steps that organic acid is added to the aqueous solution of aplatinum precursor to be stirred and dissolved, and the PH value is adjusted by using an alkali solution; activated carbon is put into the solution to be soaked; after soaking is completed, the solution is transferred to a high-pressure hydrogenated kettle, air in the hydrogenated kettle is displaced by nitrogen, hydrogen is added rapidly after the temperature is increased, and heat preservation,cooling, and pressure leakage are conducted; after filtering and washing are conducted, the platinum-carbon catalyst is obtained. According to the method, a stable macro complex is formed after the coordination of platinum salt and organic acid is conducted in the solution, the activated carbon is put into the solution to be soaked, the coordination strength of the organic acid and platinum is controlled by adjusting the PH of the solution to further control the size of the platinum complex and the distribution of the platinum complex in activated carbon pores, rapid reduction is conducted, and the platinum is condensed in medium and large pores in the activated carbon; the prepared platinum-carbon catalyst can rapidly catalyze the hydrogenation reduction of 6,9-imino ether, and the catalyst can be used for consecutive 30 times without being processed.

Description

【Technical field】 [0001] The invention relates to the technical field of preparation of azithromycin, in particular to the technical field of a preparation method of a platinum carbon catalyst for high-efficiency azithromycin synthesis. 【Background technique】 [0002] Azithromycin is a broad-spectrum macrolide antibiotic, which has a high cure rate in the treatment of respiratory tract, genitourinary tract, skin and other infections caused by bacteria. Its synthesis is obtained by rearrangement of erythromycin oxime to obtain 6,9-imine ether, reduction of 6,9-imine ether to obtain dihydrohomoerythromycin, and methylation of dihydrohomoerythromycin to obtain azithromycin. The reduction of 6,9-imine ether to dihydrohomoerythromycin is a key step in the whole synthetic route. At present, the reduction methods of 6 and 9-imine ethers are mainly divided into two types: one uses chemical reducing agents such as potassium borohydride for reduction, and the other uses noble metal c...

Claims

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Application Information

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IPC IPC(8): B01J23/42C07H1/00C07H17/00
CPCB01J23/42C07H1/00C07H17/00
Inventor 竺亚庆郑飞跃李思全
Owner 徐学军
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