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Process for preparing furaltadone hydrochloride

A kind of furaltadone hydrochloride and technology, applied in the field of organic synthesis, can solve the problems of low yield, many reaction steps, troublesome operation and the like, and achieve the effects of high yield and simplified operation

Inactive Publication Date: 2009-08-05
SHANDONG FANGXING SCI & TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The conventional manufacturing process is: hydrolyze 5-nitrofurfural diethyl ester under alkaline sodium hydroxide conditions to form 5-nitrofurfural, neutralize the solution with hydrochloric acid to neutrality, separate layers, and remove the 5-nitrofural in the lower layer The base furfural is transferred to another reaction tank, and the measured water, hydrochloric acid and morpholine methylene aminoazolone are added to the other reaction tank for condensation, and then furaltadone hydrochloride is formed by heat preservation, pressure filtration, crystallization, and centrifugal drying. , the reaction steps are many, the operation is troublesome, and the yield is low

Method used

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  • Process for preparing furaltadone hydrochloride

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Embodiment 1

[0007] (1) Put 500L water and 200kg concentration of 31% hydrochloric acid into the tank, cover the feeding port, and open the condenser cooling water; (2) Then the reaction tank jacket enters the steam, and when the temperature rises to 46°C, add 55kg5-nitrate Diethylfurfural diethyl ester, slowly heat up, 15°C per hour, when the temperature rises to 61°C, add 95kg morpholine methyleneamino azlactone (3) and continue to slowly heat up, when the temperature in the tank rises to 80°C, maintain 80--85°C temperature for 30 minutes; (4) Stop the steam after heat preservation, press filter, put the filtrate into the crystallization tank, start stirring, and cool down to 10°C; (5) Centrifuge to dry, wash with 20 kg of 95% ethanol Shake dry.

Embodiment 2

[0009] (1) Put 500L water and 200kg concentration of 31% hydrochloric acid into the tank, cover the feeding port, and open the condenser cooling water; (2) Then the reaction tank jacket enters the steam, and when the temperature rises to 48°C, add 55kg5-nitrate Diethylfurfural diethyl ester, slowly heat up, 15°C per hour, when the temperature rises to 63°C, add 95kg morpholine methyleneamino azlactone (3) and continue to slowly heat up, when the temperature in the tank rises to 80°C, maintain 80--85°C temperature for 30 minutes; (4) Stop the steam after heat preservation, press filter, put the filtrate into the crystallization tank, start stirring, and cool down to 10°C; (5) Centrifuge to dry, wash with 20 kg of 95% ethanol Shake dry.

Embodiment 3

[0011] (1) 500L water and 200kg concentration of 31% hydrochloric acid are put into the tank, cover the feeding port, and open the condenser cooling water; (2) Then the reaction tank jacket enters steam, and when the temperature is raised to 50°C, add 55kg 5- Nitrofurfural diethyl ester slowly heats up to 15°C per hour. When the temperature rises to 65°C, add 95kg morpholine methyleneamino azlactone (3) and continue to slowly heat up. When the temperature in the tank rises to 80°C, Maintain the temperature at 80--85°C for 30 minutes; (4) stop the steam after heat preservation, press filter, put the filtrate into the crystallization tank, start stirring, and cool down to 10°C; (5) spin dry in a centrifuge, wash with 20 kg of 95% ethanol Shake dry.

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Abstract

The invention belongs to the field of organic synthesis, and in particular relates to a process for manufacturing furaltadone hydrochloride. The technical proposal comprises the following step a condensation reaction of 5-nitro frfural diacetate and morpholinomethylene amino oxazolone is performed under the hydrochloric acid condition to generate the furaltadone hydrochloride, wherein the weight ratio of the 5-nitro frfural diacetate to the morpholinomethylene amino oxazolone is 55:95. The process has the advantages that the process has high yield, and the reaction yield is between 85 and 90 percent (calculated the morpholinomethylene amino oxazolone); and the process simplifies the operation, and reduces a two-step reaction to a one-step reaction.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a process for producing furaltadone hydrochloride. Background technique [0002] The trade name of furaltadone hydrochloride is: Fumozodone, and the molecular formula is C 13 h 16 N 4 o 6 .HCL.H 2 O, chemical name: 5-(4-morpholinylmethyl)-3-[(5-nitro-2-furyl)methylene]amino-2-oxazolidinone hydrochloride. It is a yellow crystalline powder in appearance. It is a broad-spectrum antibacterial drug, which is used for bacterial diseases such as poultry and for the prevention of coccidia. The conventional manufacturing process is: hydrolyze 5-nitrofurfural diethyl ester under alkaline sodium hydroxide conditions to form 5-nitrofurfural, neutralize the solution with hydrochloric acid to neutrality, separate layers, and remove the 5-nitrofural in the lower layer The base furfural is transferred to another reaction tank, and the measured water, hydrochloric acid and morpholine methy...

Claims

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Application Information

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IPC IPC(8): C07D413/12
Inventor 李秀兵叶红孙涛
Owner SHANDONG FANGXING SCI & TECH DEV
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