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Process method for preparing cefradine through microreactor

A technology of microreactor and cephradine, which is applied in the direction of organic chemistry, can solve the problems of large amount of liquid nitrogen, environmental pollution, safety hazards, etc., and achieve the effects of reducing emissions, reducing production costs, and reducing pollution

Inactive Publication Date: 2021-02-05
河北载和新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

During the whole reaction process, a large amount of liquid nitrogen is used, and at the same time, a large amount of methylene chloride is volatilized and taken away, causing environmental pollution, and there are certain safety hazards. These problems need to be solved, so it needs to be improved

Method used

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  • Process method for preparing cefradine through microreactor
  • Process method for preparing cefradine through microreactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of processing method preparing cephradine by microreactor, comprises the following steps:

[0025] S1: Preparation of mixed acid anhydride: Dissolve 55g of dihydrodecane salt, 0.3ml of pyridine, and 3.0ml of NMA in 140ml of dichloromethane, add 20ml of pivaloyl chloride after cooling down to generate mixed anhydride in mixed anhydride tank 1.

[0026] S2: Dissolution of 7-ADCA: Dissolve 40 g of 7-ADCA in 7-ADCA tank 2 in 100 ml of dichloromethane, add 30 ml of tetramethylguanidine after cooling down.

[0027] S3: The mobile phase is mixed acid anhydride with a temperature of -20°C and a flow rate of 28ml / min, and 7-ADCA with a temperature of -25°C and a flow rate of 20ml / min is used as a dispersed phase. 7-ADCA is dispersed through the membrane and microchannel The mixed acid anhydride in the mixture is mixed and reacted in the microreactor 4, and the reaction temperature is -45°C. After the reaction is completed, samples are taken from the storage tank 5 for det...

Embodiment 2

[0030] A kind of processing method preparing cephradine by microreactor, comprises the following steps:

[0031] S1: Preparation of mixed acid anhydride: Dissolve 55g of dihydrodecane salt, 0.3ml of pyridine, and 3.0ml of NMA in 140ml of dichloromethane, add 20ml of pivaloyl chloride after cooling down to generate mixed anhydride in mixed anhydride tank 1.

[0032] S2: Dissolution of 7-ADCA: Dissolve 40g of 7-ADCA in 7-ADCA tank 2 in 100ml of dichloromethane, add 30ml of tetramethylguanidine after cooling down;

[0033] S3: The mobile phase is mixed acid anhydride at a temperature of -30°C and a flow rate of 28ml / min, and the dispersed phase is 7-ADCA at a temperature of -15°C and a flow rate of 20ml / min. 7-ADCA is dispersed through the membrane and microchannel The mixed acid anhydride in the mixture is mixed and reacted in the microreactor 4, and the reaction temperature is -40°C. After the reaction, samples are taken every 1 hour for detection.

[0034] According to the ab...

Embodiment 3

[0036] A kind of processing method preparing cephradine by microreactor, comprises the following steps:

[0037] S1: Preparation of mixed acid anhydride: Dissolve 55g of dihydrodecane salt, 0.3ml of pyridine, and 3.0ml of NMA in 140ml of dichloromethane, add 20ml of pivaloyl chloride after cooling down to generate mixed anhydride in mixed anhydride tank 1.

[0038] S2: Dissolution of 7-ADCA: Dissolve 40g of 7-ADCA in 7-ADCA tank 2 in 100ml of dichloromethane, add 30ml of tetramethylguanidine after cooling down;

[0039] S3: The mobile phase is mixed acid anhydride with a temperature of -30°C and a flow rate of 75ml / min, and the dispersed phase is 7-ADCA with a temperature of -15°C and a flow rate of 50ml / min. 7-ADCA is dispersed through the membrane and microchannel The mixed acid anhydride in the mixture is mixed and reacted in the microreactor 4, and the reaction temperature is -40°C. After the reaction, samples are taken every 1 hour for detection.

[0040] According to th...

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Abstract

The invention discloses a process method for preparing cefradine through a microreactor. The process method comprises the following main raw materials: mixed anhydride and 7-ADCA. According to the process, a mixed anhydride solution with a certain temperature and a certain flow rate is used as a mobile phase, a 7-ADCA solution with a certain temperature and a certain flow rate is used as a dispersion phase, uniform and rapid mixing and reaction are performed through a membrane dispersion microreactor, and a cefradine solution is prepared. Compared with the prior art, the method has the advantages that various conditions in production can be more accurately controlled, the mass transfer rate is increased, a fine, rapid and controllable continuous production mode is achieved, the productionefficiency is improved, meanwhile, zero application of liquid nitrogen in the production process is achieved, the production cost is reduced, the discharge amount of dichloromethane is reduced, and the pollution to the environment is reduced.

Description

technical field [0001] The invention relates to the technical field of cephradine preparation, in particular to a process for preparing cephradine through a microreactor. Background technique [0002] Cephradine belongs to the first-generation cephalosporins, which is characterized by resistance to β-lactamase, has a strong bactericidal effect on drug-resistant Staphylococcus aureus Klebsiella pneumoniae, and has a strong bactericidal effect on hemolytic streptococcus, pneumococcus, Escherichia coli Bacteria and some Proteus have antibacterial effects. Clinically, it is mainly used to treat respiratory tract, urinary tract, skin, soft tissue and other infections. It has good curative effect and high safety on gastrointestinal tract infection, bone and joint infection, sepsis, endocarditis, etc., so it is extremely safe for clinical application. Widely, the synthetic technique of cephradine mainly contains enzymatic synthesis method and chemical synthesis method now, and enz...

Claims

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Application Information

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IPC IPC(8): C07D501/22C07D501/06
CPCC07D501/06C07D501/22
Inventor 刘志猛张建辉高明堂李孟华
Owner 河北载和新材料科技有限公司
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