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Method for preparing medicine and medicine intermediate through continuous solid-liquid-gas three-phase reaction

A three-phase reaction, solid-liquid-gas technology, used in the field of medicine and chemical industry

Inactive Publication Date: 2021-07-23
浙江瑞博制药有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, considering that it has not been used in a microchannel reactor to realize continuous production, it is also necessary to try to develop it to explore whether it is true that the microchannel reaction of the three-phase system is as stated in the above-mentioned journal literature. Whether the device can be applied to organic synthesis reactions, and further whether it can be applied to drug synthesis reactions, more specifically, can be applied to the drug meropenem and 10,11-dihydro-5H-dibenzo[b,f]azepine synthesis reaction

Method used

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  • Method for preparing medicine and medicine intermediate through continuous solid-liquid-gas three-phase reaction
  • Method for preparing medicine and medicine intermediate through continuous solid-liquid-gas three-phase reaction
  • Method for preparing medicine and medicine intermediate through continuous solid-liquid-gas three-phase reaction

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 30 g of the 30 g of the protective methase was dissolved in 753 ml of tetrahydrofuran, 600 ml of water and 6 g of 10% palladium carbon dry group were added, and a reaction mixture having a total mass of 1310 g was obtained, which was a homogeneous feed liquid. Using a stainless steel diaphragm pump, a stainless steel diaphragm pump is used to control the feedstock and the catalyst mixed flow rate, hydrogen flow rate, hydrogen and substrate molar ratio, temperature, pressure, and the like, the experimental results are obtained. The following table.

[0037]

[0038] Among them, the actual residence time, equal to the total liquid volume of the reaction module divided by the total flow rate (the volume flow rate of hydrogen is estimated according to the pressure and consumption).

Embodiment 2

[0040] 30 g of the 30 g of the protective methase was dissolved in 753 ml of tetrahydrofuran, 600 ml of water and 6 g of 10% palladium carbon dry group were added, and a reaction mixture having a total mass of 1310 g was obtained, which was a homogeneous feed liquid. The feed to the U-shaped microchannel reactor, control the feedstock and the catalyst mixed flow rate, hydrogen flow rate, hydrogen and substrate molar ratio, temperature, pressure, and the like, and the obtained experimental results are obtained in the following table data using a stainless steel diaphragm. The following table.

[0041]

[0042] Among them, the actual residence time, equal to the total liquid volume of the reaction module divided by the total flow rate (the volume flow rate of hydrogen is estimated according to the pressure and consumption).

Embodiment 3

[0044] 30 g 2, 2'-dinitribenzyl, 760 ml of ethanol was added 600 ml of water and 6 g of 10% palladium carbon dry group to give a reaction mixture having a total mass of 1240 g, which was a homogeneous feed liquid. The feed to the T-type microchannel reactor, control the mixed flow rate, hydrogen flow rate, hydrogen and substrate molar ratio, temperature, pressure, and the like, the experimental results are obtained in the following table. The following table.

[0045]

[0046] Among them, the actual residence time, equal to the total liquid volume of the reaction module divided by the total flow rate (the volume flow rate of hydrogen is estimated according to the pressure and consumption).

[0047]After the 2,2'-diaminobenzoenzylbenzel flowing from the microchannel reactor continues to react with the phosphoric acid, 10, 11-dihydro-5H-diphenne is obtained in the water to obtain 10,11-dihydro-5H-dibenzene [B, F] Nazo Zhuo Zhuo Zhuo Zhuo Continuing production is achieved compared ...

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Abstract

The invention provides a method for preparing meropenem or 10, 11-dihydro-5H-dibenzo [b, f] azepine through continuous solid-liquid-gas three-phase reaction, which comprises the following steps of pumping a reaction material dissolved with a catalyst into a microchannel reactor by using a diaphragm pump, and blowing hydrogen into the microchannel reactor by using the pressure of a steel cylinder. According to the method, the continuous production of meropenem or 10, 11-dihydro-5H-dibenzo [b, f] azepine is realized by using a microchannel reactor. The technical effects of short reaction time, thorough reaction degree and high product yield are achieved.

Description

Technical field [0001] The present invention belongs to the field of medicine and chemical chemical, and is specifically related to the preparation of drug and drug intermediates, which specifically in the pharmaceutical intermediate, specifically metobenne, and [b, f] aza. Zhuo method. Background technique [0002] Microchannel reactor in Journal documents 2004, Volume 23, 5th Chemical Progress, "Microspactics Research and Prospect", the microenactor has a large reactor in the chemical and chemical industry, the high reactor cannot match the superiority, performance at temperature Control, reactor volume, conversion rate and yield, ensure safety, easy to enlarge. [0003] Further, in the 2008, the application of "microchannel reactor in the synthesis reaction". "" "" "" "" "" "" "" "" "" "" "" "" "" "" "" "" "" "" " A cross-type channel microreactor cross-crossing cross-channel crossover is used in catalytic hydrogenation reactions of cyclohexene. 64 parallel channels were used ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D477/20C07D477/06C07D223/22
CPCC07D223/22C07D477/06C07D477/20Y02P20/582
Inventor 位军辉金明辉张辉孙文兵陈云青朱国良李原强林建广
Owner 浙江瑞博制药有限公司