Method for preparing rifampicin by utilizing cascade reaction of kettle type reaction device and microchannel reaction device

A technology of microchannel reaction and reaction device, which is applied in chemical instruments and methods, chemical/physical/physical chemical reactors, chemical/physical/physical chemical processes, etc. Achieve the effect of saving raw material cost, short reaction time and low cost

Inactive Publication Date: 2017-05-10
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since 1-methyl-4-amino-piperazine is relatively expensive, costs have a greater impact on revenue

Method used

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  • Method for preparing rifampicin by utilizing cascade reaction of kettle type reaction device and microchannel reaction device
  • Method for preparing rifampicin by utilizing cascade reaction of kettle type reaction device and microchannel reaction device

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Take rifamycin S sodium salt (42g, 0.0584mol) with a purity of 95% and place it in a three-necked flask A, add 70mL N,N-dimethylformamide and sulfuric acid (2.84mL, 0.0533mol), and stir at room temperature for 45min , the reaction solution was filtered; after the filtration was completed, the filtrate was placed in a three-necked beaker bottle B, dimethylol terbutylamine (9.86mL, 0.0759mol) was added, and stirred at 45°C for 2h; 1-methyl-4- Amino-piperazine (10mL, 0.086mol) was placed in a three-necked flask C, and 193mL of N,N-dimethylformamide was added, and stirred to form a homogeneous solution; pump A was used to extract acetic acid and N,N with a volume ratio of 1:100 -The mixture of dimethylformamide, the flow rate is 0.0436mL / min, the reaction solution in the three-necked flask B is directly extracted by the pump B, the flow rate is 0.623mL / min, and the two are mixed with a T-type mixing valve; Extract the liquid in the three-necked flask C at a flow rate of 1.3...

Embodiment 2

[0034] Take rifamycin S sodium salt (42 g, 0.0584 mol) with a purity of 95% and place it in a three-necked flask A, add 70 mL N, N-dimethylformamide and sulfuric acid (2.84 mL 0.0533 mol), and stir at room temperature for 45 min. The reaction solution was filtered; after the filtration was completed, the filtrate was placed in a three-necked beaker bottle B, dimethylol terbutylamine (9.86mL 0.0759mol) was added, and stirred at 45°C for 2h; 10mL 0.086mol1-methyl-4- Amino-piperazine was placed in a three-necked flask C, and 193mL N,N-dimethylformamide was added, and stirred to form a homogeneous solution; pump A pumped acetic acid and N,N-dimethylformamide with a volume ratio of 1:100 The mixture, the flow rate is 0.117mL / min, the reaction solution in the three-necked flask B is directly extracted by the pump B, the flow rate is 1.68mL / min, and the two are mixed with a T-shaped mixing valve; the reaction solution in the three-necked flask C is directly extracted by the pump C Th...

Embodiment 3

[0036] Take rifamycin S sodium salt (42g, 0.0584mol) with a purity of 95% and place it in a three-necked flask A, add 70mL N,N-dimethylformamide and (2.84mL 0.0533mol) sulfuric acid, and stir at 40°C for 1h , filter the reaction solution; after the filtration is completed, put the filtrate into a three-necked beaker bottle B, add (9.86mL 0.0759mol) dimethylol terbutylamine, and stir at 45°C for 2h; add 10mL0.086mol 1-methyl- 4-Amino-piperazine was placed in a three-necked flask C, and 193mL N,N-dimethylformamide was added, and stirred to form a homogeneous solution; pump A was used to extract acetic acid and N,N-dimethylformamide with a volume ratio of 1:100 A mixture of formamide, the flow rate is 0.0436mL / min, the reaction solution in the three-necked flask B is directly extracted by the pump B, the flow rate is 0.623mL / min, and the two are mixed with a T-shaped mixing valve; the three-necked flask C is directly extracted by the pump C The liquid in the medium, with a flow r...

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Abstract

The invention provides a method for preparing rifampicin by utilizing cascade reaction of a kettle type reaction device and a microchannel reaction device. In the kettle type reaction device, rifamycin S sodium salt is used as a raw material to obtain N-tedin-1,3-oxazine (5,6-C) rifamycin through reaction, and the N-tedin-1,3-oxazine (5,6-C) rifamycin reacts with 1-methyl-4-amino-piperazine in the microchannel reaction device to obtain the rifampicin. Continuous production of the rifampin is achieved, the product quality is good, the cost is low, the profit is high, and the method is green, environmentally friendly, capable of saving energy, efficient and suitable for industrial application.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing rifampicin by serial reaction of a kettle type reaction device and a microchannel reaction device. Background technique [0002] Rifampicin was invented in 1965. The discovery of rifampicin brought about a major leap forward in the treatment of tuberculosis. Some experts spoke highly of the anti-tuberculosis effect of rifampicin and believed that the anti-tuberculosis treatment has now entered the era of rifampicin. , and believed that tuberculosis, which used to be treated with surgery, could be controlled without surgery with rifampicin. [0003] In the "preparation method of high-quality rifampicin" disclosed in Chinese patent 101486716A, rifamycin S sodium salt first generates N-tertidine-1,3-oxazine (5,6-C) rifamycin, and then with 1-Methyl-4-amino-piperazine reacts to form rifampicin. Due to the different solvents of the react...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D498/08B01J19/00
CPCC07D498/08B01J19/0093
Inventor 郭凯黄思宇李昕张锴
Owner NANJING UNIV OF TECH
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