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Preparation method for rifampin by using micro-reaction apparatus

A technology of micro-reaction device and micro-reactor, which is applied in the direction of organic chemistry, can solve the problems of unsatisfactory product quality of rifampicin, and achieve the effect of high-efficiency heat and mass transfer capacity, good product quality and large specific surface area

Active Publication Date: 2014-02-26
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method produces the quality of rifampicin product not ideal enough

Method used

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  • Preparation method for rifampin by using micro-reaction apparatus
  • Preparation method for rifampin by using micro-reaction apparatus

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In the microchannel reaction device, the diameter of the connecting pipe is 2.1mm, the length of the inlet pipe is 15cm, the length of the connecting pipe between the T-shaped valve and the microchannel reactor is 25cm, and the length of the connecting pipe between the microreactor and the outlet is 20cm; the volume of the microchannel reactor is 5ml.

[0026] 1. Take 10.75g of rifamycin oxazine, stir it into a homogeneous phase with DMF at room temperature, and obtain a mixed solution volume of 25mL; 2. Take 0.80g of 1-methyl-4-nitropiperazine with a pipette gun, add DMF to dilute to 25mL. The two materials are mixed and pumped into the microchannel reactor through the T-valve. The two reaction fluids flow through the microreactor at 0.5mL / min, the reaction molar ratio of rifamycin oxazine and 1-methyl-4-nitropiperazine is 1:1, and the reactor temperature is 40°C. The reaction residence time was 5 min, and the crude product was collected at the outlet; the conversion...

Embodiment 2

[0028] The microchannel reactor is basically the same as Example 1, and the difference is only: the pipeline diameter of this microchannel reactor is 2.1mm, and the length of the liquid inlet pipe is 10cm, and the connecting pipe length between the inlet and the microreactor The length of the connecting tube between the microreactor and the outlet is 30cm; the volume of the microchannel reactor is 4ml.

[0029] 1. Take 10.75g of rifamycin oxazine, stir it with tetrahydrofuran at room temperature to form a homogeneous phase, and the volume of the mixed solution is 30mL; 2. Take 0.80g of 1-methyl-4-nitropiperazine with a pipette gun, add tetrahydrofuran to dilute to 30mL. The materials are mixed and pumped into the microchannel reactor through the T-valve. The two reaction fluids flowed through the microreactor at 0.4mL / min, the reaction molar ratio of rifamycin oxazine and 1-methyl-4-nitropiperazine was 1:1, and the reactor temperature was 50°C. The reaction residence time wa...

Embodiment 3

[0031] The microchannel reactor is basically the same as Example 1, and the difference is only: the pipeline diameter of this microchannel reactor is 1.6mm, and the liquid inlet pipe length is 8cm, and the connecting pipe length between the inlet and the microreactor The length of the connecting tube between the microreactor and the outlet is 25cm; the volume of the microchannel reactor is 6mL.

[0032] 1. Take 10.75g of rifamycin oxazine, stir it with acetic acid at room temperature to form a homogeneous phase, and the volume of the mixed solution is 20mL; 2. Take 0.80g of 1-methyl-4-nitropiperazine with a pipette gun, add acetic acid to dilute to 20mL. The materials are mixed and pumped into the microchannel reactor through the T-valve. The two reaction fluids flowed through the microreactor at 0.4mL / min, the reaction molar ratio of rifamycin oxazine and 1-methyl-4-nitropiperazine was 1:1, and the reactor temperature was 60°C. The reaction residence time was 6.25 min. The...

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Abstract

The invention discloses a preparation method for rifampin by using a micro-reaction apparatus. The method comprises the following steps (1) dissolving rifamycin oxazine in an organic solvent so as to obtain a homogeneous solution; (2) dissolving 1-methyl-4-nitropiperazine in an organic solvent so as to obtain a homogeneous solution; (3) respectively pumping the two homogeneous solutions obtained in the step (1) and the step (2) into the micro-reaction apparatus; and (4) collecting outflowing liquid which is a crude rifampin product. A micro-reactor has the characteristics of a great specific surface area, a high transmission rate, short contact time, a few by-products, strong heat transfer and mass transfer capability, rapid and direct amplification, high security, good operationality and the like. A micro-reaction system is a parallel system of a modular structure and has the characteristic of good portability; the system can be dispersively constructed in a place where a product is used and realizes on-site production and product supply, so portability of a chemical plant is realized indeed; moreover, production can be adjusted by increasing or decreasing channel numbers and replacing modules according to market conditions, so the system has high operational flexibility.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing anti-tuberculosis drug rifampicin by using a micro-reaction device. Background technique [0002] Rifampicin was invented in 1965, and the discovery of rifampicin brought another great leap forward in the treatment of tuberculosis. Some experts spoke very highly of the anti-tuberculosis effect of rifampicin, and believed that the anti-tuberculosis treatment has entered rifampicin now. He believed that tuberculosis, which used to be treated with surgery, could be controlled without surgery with rifampicin. [0003] In Chinese patent 1045993A, "a preparation method of rifamycin sodium salt S" is disclosed, which uses ferric oxide oxidation method under acidic conditions to prepare rifamycin S. Salt-forming reaction is carried out by sodium method, and rifamycin sodium salt is prepared under the condition of pH 8.5-10.5. Because the us...

Claims

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Application Information

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IPC IPC(8): C07D498/08
CPCC07D498/08
Inventor 郭凯李昕陈安邦张凯
Owner NANJING UNIV OF TECH
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