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A kind of method utilizing microchannel reaction device to prepare rifampicin

A technology of channel reaction device and microchannel reaction, which is applied in the direction of organic chemistry, can solve the problems of high price and the impact of cost on income, and achieve the effects of short reaction time, saving raw material costs, low toxicity and pollution

Active Publication Date: 2021-04-30
NANJING TECH UNIV
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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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  • A kind of method utilizing microchannel reaction device to prepare rifampicin
  • A kind of method utilizing microchannel reaction device to prepare rifampicin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Get 10g of 97% rifamycin S and 3.75ml of 99.5% by mass concentration of acetic acid and 10ml of 98% of 98% purity and mix it with 25ml of homogeneous liquid A; N, N-dimethylol terbutylamine with a purity of 98% in ml becomes a homogeneous liquid B without adding a solvent; 2.31 ml of 1-amino-4-methylpiperazine with a purity of 98% and 22.5 ml of a purity of 98 % N,N-dimethylformamide mixed into 25ml of homogeneous liquid C; 1L of distilled water was taken as homogeneous liquid D; homogeneous liquid A was extracted by pump A at a flow rate of 0.885mL / min, and homogeneous liquid was extracted by pump B Phase liquid B, the flow rate is 0.115mL / min, the two are fully mixed with an inverted Y-shaped mixing valve, and then pumped into the microchannel reactor I together, the volume of the microchannel reactor is 20ml, the reaction temperature is 75°C, and the reaction time is 20min , the outflowing reaction solution is a mixed liquid of N-tertidine-1,3-oxazine (5,6-C) rifamyc...

Embodiment 2

[0040] Get 10g of rifamycin S with a purity of 97% and 3.75ml of acetic acid with a concentration of 99.5% by mass and 10ml of a purity of 98% N,N-dimethylformamide and mix it with 25ml of homogeneous liquid A; take 3.2 N,N-dimethylol terbutylamine with a purity of 98% in ml and N,N-dimethylformamide with a purity of 97ml are mixed to form 100ml of homogeneous liquid B; Mix 1-amino-4-methylpiperazine with 22.5ml of N,N-dimethylformamide with a purity of 98% to form 25ml of homogeneous liquid C; take 1L of distilled water as homogeneous liquid D; Liquid A, the flow rate is 0.2mL / min, the homogeneous liquid B is extracted by the pump B, the flow rate is 0.8mL / min, the two are fully mixed with an inverted Y-shaped mixing valve, and then pumped into the microchannel reactor I together, the microchannel reaction The volume of the device is 20ml, the reaction temperature is 75°C, and the reaction time is 20min. Formamide mixed liquid, the actual molar ratio of rifamycin S and N,N-d...

Embodiment 3

[0042] Get 10g of rifamycin S with a purity of 97% and 7.5ml of mass percent concentration as 99.5% acetic acid and 14ml of 98% purity N, N-dimethylformamide mixed to be 25ml of homogeneous liquid A; take 2.44 N, N-dimethylol terbutylamine with a purity of 98% in ml becomes a homogeneous liquid B without solvent; 2.12 ml of 1-amino-4-methylpiperazine with a purity of 98% and 22.5 ml of a purity of 98 % N,N-dimethylformamide mixed into 25ml of homogeneous liquid C; 1L of distilled water was taken as homogeneous liquid D; homogeneous liquid A was extracted by pump A at a flow rate of 0.885mL / min, and homogeneous liquid was extracted by pump B Phase liquid B, the flow rate is 0.115mL / min, the two are fully mixed with an inverted Y-shaped mixing valve, and then pumped into the microchannel reactor I together, the volume of the microchannel reactor is 20ml, the reaction temperature is 75°C, and the reaction time is 20min , the outflowing reaction solution is a mixed liquid of N-ter...

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Abstract

The invention discloses a method for preparing rifampicin by using a microchannel reaction device. Through a microchannel reactor, rifamycin S is used as a raw material to undergo cyclization, hydrolysis, condensation and crystallization processes without post-treatment process, and directly obtains Rifampicin crude. The invention realizes complete continuous production of rifampicin, has high yield, low cost, high profit, environmental protection, energy saving and high efficiency, and is 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 using 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 rifampin" disclosed in Chinese patent 101486716A, rifamycin S sodium salt first generates N-tertidine-1,3-oxazine (5,6-C) rifamycin, and then 1-Methyl-4-amino-piperazine reacts to form rifampicin. Due to the different solvents of the reaction, it is necessary to obtain the crude product of N-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D498/08
CPCC07D498/08
Inventor 郭凯李昕黄思宇齐豪苗珊珊
Owner NANJING TECH UNIV
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