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A kind of preparation method of nitrofurantoin

A technology of nitrofurantoin and purified water, which is applied in the field of nitrofurantoin preparation, can solve the problems of high energy consumption and low yield, and achieve the effects of improved catalyst activity, high product purity and improved conversion rate

Active Publication Date: 2020-07-07
HUNAN XIANGYIKANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The primary purpose of the present invention is to provide a new preparation method of nitrofurantoin in order to overcome the deficiencies in the prior art, which can overcome the problems of low yield, high energy consumption and high impurities contained in the product in the existing nitrofurantoin preparation method. without risk of harming the human body

Method used

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  • A kind of preparation method of nitrofurantoin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 5kg of 10% hydrochloric acid and 30kg of purified water into a reactor equipped with a reverse osmosis membrane, heat to 60°C, add 7kg of 5-nitrofurfural diethyl ester, heat up to 80°C, and wait for 5-nitrofurfural diethyl ester to be hydrolyzed Completely, add iron-nickel combination catalyst and 42g of sodium chloride solid, then add 30kg of aminohydantoin that has been preheated to 60°C, heat up to 90°C and reflux, keep warm for 40min, and then wash the reactant with purified water until the pH is 6.0, shake off the dry matter, wash the obtained nitrofurantoin with 90°C flowing purified water for 20min, cool to 0°C, and obtain 6.67kg of finished nitrofurantoin containing nitrofural with a content of 0.002% and 0.03% of 5-nitrofurfural diethyl ester. The rate is 97.3%.

Embodiment 2

[0025] Add 10kg of 20% hydrochloric acid and 80kg of purified water into a reactor equipped with a reverse osmosis membrane, heat to 65°C, add 20kg of 5-nitrofurfural diethyl ester, heat up to 82°C, and wait for 5-nitrofurfural diethyl ester to be hydrolyzed Completely, add iron-nickel catalyst and 150g of sodium chloride solid, then add 80kg of aminohydantoin that has been preheated to 65°C, heat up to 92°C and reflux, keep warm for 50min, and then wash the reactant with purified water until the pH is 6.5 , shake off the dry matter, wash the gained nitrofurantoin with 92 DEG C of flowing purified water for 30 min, cool to 5 DEG C, and obtain 19.73 kg of finished product Nitrofuraltoin containing nitrofurazone content of 0.001% and 0.02% of 5-nitrofurfural diethyl ester, the yield is 98.1%.

Embodiment 3

[0027] Add 5kg of 10% hydrochloric acid and 40kg of purified water into a reactor equipped with a reverse osmosis membrane, heat to 65°C, add 10kg of 5-nitrofurfural diethyl ester, heat up to 85°C, and wait for 5-nitrofurfural diethyl ester to be hydrolyzed Complete, add iron-nickel-copper combination catalyst and 100g sodium chloride solid, then add 50kg of aminohydantoin that has been preheated to 65°C, heat up to 95°C and reflux, keep warm for 60min, and then wash the reactant with purified water to pH 7.0, shake off the dry material, and the gained nitrofurantoin is washed with 94 DEG C of flowing purified water for 30 min, cooled to 0 DEG C, and the obtained nitrofurantoin content is 0.001%, 0.01% of nitrofural diethyl ester 9.70kg of finished product nitrofural. The rate is 99.0%.

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Abstract

The invention discloses a preparation method of nitrofurantoin. The technical solution is: add hydrochloric acid and purified water into the reaction device installed with reverse osmosis membrane, heat up to 60°C-70°C, add 5-nitrofurfural diethyl ester, maintain 80°C-85°C for complete hydrolysis, add catalyst and appropriate amount Sodium chloride solid, then add aminohydantoin preheated to 60°C-70°C, pressurize, maintain the temperature at 90°C-95°C and reflux, keep warm for 40min-60min, wash the reaction product with purified water until the pH is 6.0 to 8.0, shake off the dry material, and wash the obtained nitrofurantoin with flowing purified water at 90°C to 95°C for a certain period of time to obtain the finished nitrofurantoin. The production rate of nitrofurantoin is effectively improved, the production energy consumption is reduced, the amount of impurities in nitrofurantoin is greatly reduced, and the pharmaceutical standard is met.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a preparation method of nitrofurantoin. Background technique [0002] Nitrofurantoin, also known as nitrofurantoin, nitrofurantoin, nitrofurantoin, nitrofurantoin, chemical name 1-[[(5-nitro-2-furanyl)methylene]amino]-2,4 -imidazolidinedioe, molecular formula C 8 h 6 N 4 o 5 , 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. Clinically, it is often used for urinary system infections caused by sensitive bacteria, such as pyelonephritis and urinary tract infections. Cystitis and prostatitis etc. [0003] The existing synthetic route of the drug mainly prepares acetone semicarbazone from hydrazine hydrate, urea and acetone, and then from acetone semicarbazone and sodium methoxide. Hy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D405/12
CPCC07D405/12
Inventor 帅放文王向峰章家伟
Owner HUNAN XIANGYIKANG PHARMA