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Cistofuran synthesis and purification method

A technology of nitrofurantoin and refining method, which is applied in the field of nitrofurantoin synthesis and refining, and can solve problems such as non-compliance with customers and high residual content

Inactive Publication Date: 2009-06-10
SHANDONG FANGXING SCI & TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The residual content of nitrofural and 5-nitrofural diethyl ester in the nitrofurantoin produced by the prior art is relatively high, and the content of nitrofural in general products is 0.04% to 0.08%, and the content of 5-nitrofural diethyl ester reaches 1.0% to 2.0% , does not meet the requirements of some customers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] Add 50Kg of hydrochloric acid (30%) and 400Kg of tap water into the reaction tank first, raise the temperature to 65°C, add 70Kg of weighed 5-nitrofurfural diethyl ester, continue to raise the temperature, maintain 75°C for hydrolysis, and check the 5-nitrofural in due course. Whether diethyl furfural is completely dissolved. After the hydrolysis of diethyl 5-nitrofurfural is complete, press 410Kg of aminohydantoin preheated at 61°C into the condensation tank, continue to heat up to 90.5°C, and keep it warm for 50 minutes. Not lower than 88°C, cool down to 60°C with jacketed cooling water, return the material 5-6 times to discard the heterochromatic spots, open the bottom valve of the tank and discharge the material to the filter tank, wash with tap water until the pH is 6.5-7.5, and dry Discharging to obtain 62Kg of nitrofurantoin (dry product), put the obtained nitrofurantoin and DMF (weight ratio) in a ratio of 1:2 and add 124Kg of DMF into the reaction tank, heat up ...

Embodiment 2

[0010] Add 50Kg of hydrochloric acid (30%) and 400Kg of tap water into the reaction tank first, raise the temperature to 70°C, add 70Kg of weighed 5-nitrofurfural diethyl ester, continue to heat up, maintain 80°C for hydrolysis, and check the 5-nitrofural in due course. Whether diethyl furfural is completely dissolved. After the hydrolysis of diethyl 5-nitrofurfural is complete, press 420Kg of aminohydantoin preheated at 62°C into the condensation tank, continue to heat up to 92°C, and keep it warm for 55 minutes. Not lower than 88°C, cool down to 60°C with jacketed cooling water, return the material 5-6 times to discard the heterochromatic spots, open the bottom valve of the tank and discharge the material to the filter tank, wash with tap water until the pH is 6.5-7.5, and dry Discharging to obtain 62.5Kg of nitrofurantoin (dry product), put the obtained nitrofurantoin and DMF (weight ratio) in a ratio of 1:2 and add DMF125Kg into the reaction tank, raise the temperature to 9...

Embodiment 3

[0012] Add 50Kg of hydrochloric acid (30%) and 400Kg of tap water into the reaction tank first, raise the temperature to 68°C, add 70Kg of weighed 5-nitrofurfural diethyl ester, continue to heat up, maintain 78°C for hydrolysis, and check the 5-nitrofural in due course Whether diethyl furfural is completely dissolved, after the hydrolysis of diethyl 5-nitrofurfural is complete, press 450Kg of aminohydantoin preheated at 65°C into the condensation tank, continue to heat up to 91°C, keep warm for 60 minutes, and keep warm for 60 minutes. Not lower than 88°C, cool down to 60°C with jacketed cooling water, return the material 5-6 times to discard the heterochromatic spots, open the bottom valve of the tank and discharge the material to the filter tank, wash with tap water until the pH is 6.5-7.5, and dry Discharge, obtain nitrofurantoin 64Kg (dry product), add gained nitrofurantoin and DMF (weight ratio) by the ratio of 1:2 and add DMF128Kg and drop into the reaction tank, heat up ...

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Abstract

The invention discloses a method for synthesizing and refining nitrofurantoin and belongs to the field of chemical synthesis. The invention adopts a technical proposal that: hydrochloric acid and water are placed in a retort, heated to be between 65 and 70 DEG C, added with 5-nitrofurfural diacetate and kept at between 75 and 80 DEG C for hydrolyzation; after the 5-nitrofurfural diacetate is completely hydrolyzed, aminohydantoin preheated to be between 60 and 65 DEG C is pressed into a condensation tank, heated to be between 90 and 92 DEG C and kept at the temperature for 50 to 60 minutes; a valve on the bottom of the tank is opened to discharge materials to a filter tank; the materials are washed with running water till the pH value reaches 6.5 to 7.5; the materials are dried by spinning and discharged; and the obtained nitrofurantoin and DMF are placed into the retort according to a ratio (by weight) of 1:2 and heated to be between 85 DEG C and 90 DEG C and thus the nitrofurantoin is obtained. The method reduces the content of nitrofural in the nitrofurantoin to less than 0.01 percent, reduces the content of 5-nitrofurfural diacetate in the nitrofural to less than 1.0 percent and meets the requirements of special users.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a method for synthesizing and refining nitrofurantoin. Background technique [0002] Nitrofurantoin, also known as nitrofurantoin, the common name in English is Nitrofurantoin, and the chemical name is 1-[[(5-nitro-2-furanyl)methylene]amino]-2,4-imidazolidinedione. It was developed by Norwich Eaton Pharmaceutical Company in the United States and was established in 1953 Listed in the United States. Nitrofurantoin is a synthetic antibacterial drug with a broad antibacterial spectrum, and has antibacterial effects on most Gram-positive and negative bacteria, such as Staphylococcus aureus, Escherichia coli, Staphylococcus albus and Streptococcus pyogenes. It is clinically used for urinary system infection caused by sensitive bacteria, such as pyelonephritis, urinary tract infection, cystitis and prostatitis, etc. [0003] The production route usually adopted by the drug is to prep...

Claims

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Application Information

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IPC IPC(8): C07D405/12
Inventor 李秀兵张峰
Owner SHANDONG FANGXING SCI & TECH DEV
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