Method for continuous production and preparation of rifampicin from rifamycin S sodium salt

A technology of rifamycin and sodium salt, which is applied in the field of chemical synthesis, can solve the problems of high price and impact on income, and achieve the effects of short reaction time, reduced side reactions, low toxicity and pollution

Inactive Publication Date: 2017-05-31
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 still have a greater impact on revenue

Method used

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  • Method for continuous production and preparation of rifampicin from rifamycin S sodium salt
  • Method for continuous production and preparation of rifampicin from rifamycin S sodium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 42g 0.0584mol of rifamycin S sodium salt with a purity of 95% and place it in a three-necked flask A, add 70mL (0.908mol) of N,N-dimethylformamide and 2.84mL of 0.0533mol of sulfuric acid, stir at room temperature for 45min, and then Filter the reaction liquid; after the filtration is completed, put the filtrate in a three-necked beaker bottle B, add 9.86mL (0.0759mol) dimethylol terbutylamine, and stir at 45°C for 2h; After fractional distillation, 70% of the reaction solution was evaporated, then 70mL N,N-dimethylformamide was added and stirred to form a homogeneous solution; then 10mL0.086mol 1-methyl-4-amino-piperazine was placed in three In flask C, add 193mL N,N-dimethylformamide, stir to form a homogeneous solution; pump A to extract the reaction solution in the three-necked flask B at a flow rate of 0.666mL / min, and pump B to directly extract the reaction solution in the three-necked flask C Solution, the flow rate is 1.333mL / min, the two are mixed together...

Embodiment 2

[0031] Take 42g0.0584mol of rifamycin S sodium salt with a purity of 95% and place it in a three-necked flask A, add 70mL (0.908mol) of N,N-dimethylformamide and 1.55mL (0.0292mol) of sulfuric acid, and stir at room temperature for 45min , 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; the reaction solution -0.08 to -0.1mpa, Fractional distillation at 80°C, after distilling off 70% of the reaction solution, add 70mL N,N-dimethylformamide, stir to form a homogeneous solution (0.584mol / l); then add 10mL0.086mol 1-methyl-4- Amino-piperazine was placed in the three-necked flask C, and 193mL N,N-dimethylformamide was added, and stirred to form a homogeneous solution; B directly extracts the solution in the three-necked flask C at a flow rate of 1.333mL / min, mixes the two with a T-shaped mixing valve and pumps them together into the micror...

Embodiment 3

[0033] Take 42g 0.0584mol of rifamycin S sodium salt with a purity of 95% and place it in a three-necked flask A, add 51.3mL (0.666mol) of N,N-dimethylformamide and 2.84mL of 0.0533mol of sulfuric acid, and stir at room temperature for 45min. Filter the reaction liquid; 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; Fractional distillation at ℃, after distilling off 62.5% of the reaction solution, add 70mL N,N-dimethylformamide, stir to form a homogeneous solution; then place 10mL0.086mol 1-methyl-4-amino-piperazine in In the last flask C, add 193mL N,N-dimethylformamide and stir to form a homogeneous solution; the reaction solution in the three-necked flask B is extracted by the pump A at a flow rate of 0.666mL / min, and the pump B directly extracts the reaction solution in the three-necked flask C solution, the flow rate is 1.333mL / min, the two are mixed togethe...

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Abstract

The invention provides a method for continuous production and preparation of rifampicin from a rifamycin S sodium salt. The continuous production of the rifampicin is achieved by taking rifamycin sodium salt, dihydroxymethyl tert-butyl amine, 1-methyl-4-amino-piperazine as raw materials, and connecting a tank reactor with a microreactor in series. Compared with the prior art, the method provided by the invention achieves continuous production of the rifampicin, the steps of solvent replacement during reaction, solid precipitation and the like are omitted, raw materials and heat energy are greatly saved, the cost is saved, and profits are increased. Meanwhile, according to the method provided by the invention, the characteristics high-efficiency heat transferring capability and easy and direct amplification of a microchannel reactor are utilized, and on the premise that 1 / 3 of the raw material, namely 1-methyl-4-amino-piperazine, is reduced, the conversion rate of the rifampicin is high and reaches 85% or above, the product quality is good, and the energy consumption is low, so that the method is an environmentally friendly and efficient method for synthesizing the rifampicin, and is suitable for industrial production.

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 Chinese patent 101486716A, which discloses "preparation method of high-quality rifampicin", rifamycin S sodium salt generates N-tertidine-1,3-oxazine (5,6-C) rifamycin and N- Terbutin-1,3-oxazine (5,6-C) rifamycin generates rifampicin in two steps. Due to the different solvents of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D498/08
CPCC07D498/08
Inventor 郭凯李昕黄思宇张锴
Owner NANJING UNIV OF TECH
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