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Method for producing cistofuran large particle crystal

A technology for nitrofurantoin and a production method, which is applied in the field of nitrofurantoin large particle crystal production, can solve the problems of affecting product yield and cost, increasing operation time and difficulty, material loss and the like, and achieving the effect of facilitating material rejection

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 crystallization of obtained nitrofurantoin is relatively fine, and the particle size of 95% of the products is less than 140 mesh, which is not easy to be separated by filtration, which increases the operation time and difficulty, and easily causes material loss, which affects the product yield and cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Add 50Kg of hydrochloric acid (30%) and 400Kg of tap water into the reaction tank first, heat up to 65℃, add 70Kg of 5-nitrofurfural diethyl ester, continue to heat up, maintain 75℃ for hydrolysis, and check 5-nitro in time Whether the diethyl furfural is completely dissolved, after the hydrolysis of 5-nitrofurfural diethyl is complete, press 408Kg of aminohydantoin preheated at 60°C into the condensation tank, continue to heat up to 90°C, keep the temperature for 50 minutes, and finish the temperature Not lower than 88°C, cool the cooling water to 60°C with the jacket open, return the material 5-6 times to discard the heterochromatic point, open the tank bottom valve to discharge the material to the filter tank, wash with tap water to pH 6.5-7.5, spin dry Discharge, get nitrofurantoin 63Kg (dry product), put the obtained nitrofurantoin and DMF (weight ratio) into the reaction tank in a ratio of 1:2, heat up to 86℃, keep stirring for 10 minutes, stir and open the jacket to ...

Embodiment 3

[0013] Put 50Kg of hydrochloric acid (30%) and 400Kg of tap water into the reaction tank first, heat up to 68℃, add 70Kg of weighed 5-nitrofurfural diethyl ester, continue to heat up, maintain 78℃ for hydrolysis, and check 5-nitro in time Whether the diethyl furfural is completely dissolved, after the 5-nitrofurfural diethyl ester is hydrolyzed, 450Kg of aminohydantoin preheated at 62°C is pressed into the condensation tank, and the temperature is continued to 91°C, and the temperature is kept for 55 minutes. The temperature is not lower than 88°C, the cooling water is cooled to 60°C when the jacket is opened, the material is recycled 5-6 times to discard the heterochromatic point, the bottom valve of the tank is opened and the material is discharged to the filter tank, washed with tap water until the pH is 6.5-7.5, and shaken Dry out the material to obtain 63.5Kg of nitrofurantoin (dry product). Put the obtained nitrofurantoin and DMF (weight ratio) into the reaction tank at a ra...

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PUM

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Abstract

The invention relates to a method for producing large-grained nitrofurantoin crystals, and belongs to the field of chemical synthesis. The invention adopts a technical proposal which comprises: placing a crude product of nitrofurantoin formed by the condensation of raw materials of 5-nitrofurfural diacetate and 1-aminohydantoin, and DMF of which the weight is two times of that of the crude product of the nitrofurantion in a retort, heating the mixture to between 85 and 90 DEG C, stirring the mixture, maintaining the temperature for 10 minutes, stirring the mixture, opening a clamping sleeve, cooling the retort by cooling water for 80 to 90 minutes to between 30 and 35 DEG C, stopping stirring, standing the retort for 2.5 to 3 hours to less than 2 DEG C below zero, casting material, and washing the material with 95 percent ethanol to obtain odorless DMF. Nitrofurantoin crystals prepared by the process are larger and the granularity of 95 percent of the products is more than 80 meshes, so the process facilitates filtration and separation and contributes to the reduction of production cost.

Description

Technical field [0001] The invention belongs to the field of chemical synthesis, and is specifically a method for producing nitrofurantoin large-particle crystals. Background technique [0002] Nitrofurantoin is also known as nitrofurantoin, the English generic name is Nitrofurantoin, and the chemical name is 1-[[(5-nitro-2-furanyl)methylene]amino]-2,4-imidazolidinedione. It was developed by the Norwich Eaton Pharmaceutical Company in the United States. Listed in the United States. Nitrofuranto is a synthetic antibacterial drug, which has a broad antibacterial spectrum, and has antibacterial effects on most Gram-positive and negative bacteria, such as Staphylococcus aureus, Escherichia coli, Staphylococcus albicans and Streptococcus pyogenes. It is clinically used for urinary system infections caused by sensitive bacteria, such as pyelonephritis, urinary tract infection, cystitis and prostatitis. [0003] The drug’s usual production route is to prepare acetone semicarbazone from ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D405/12
Inventor 李秀兵仇法健
Owner SHANDONG FANGXING SCI & TECH DEV
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