Method for applying formic acid glycol ester in metronidazole production, device for achieving method and method for applying device

A technology of glycol ester and formate, applied in the direction of organic chemistry, etc., can solve the problem that the utilization rate of ethylene oxide does not exceed 25%, and achieve the effect of reducing the amount of formic acid and saving production costs

Pending Publication Date: 2018-03-30
HUANGGANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above-mentioned three patents have increased the chance of contact reaction between ethylene oxide and materials to varying degrees, the utilization rate of ethylene oxide is still no more than 25%.

Method used

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  • Method for applying formic acid glycol ester in metronidazole production, device for achieving method and method for applying device
  • Method for applying formic acid glycol ester in metronidazole production, device for achieving method and method for applying device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Step 1): Add 2-methyl-5-nitroimidazole into the reaction kettle 20, add dropwise formic acid solvent with a concentration of 85% to dissolve 2-methyl-5-nitroimidazole, and add cyclic Oxyethane, add sulfuric acid with a concentration of 98% at the same time, raise the temperature to 85-95°C, and react for 1h to obtain a hydroxylated solution;

[0063] Step 2): close the reflux valve 51, open the outlet valve 71, add methanol, control the temperature within a range below 10°C higher than the boiling point of methyl formate, carry out esterification reaction, distill, and condense the steam that evaporates to obtain methyl formate , and collected by the light component liquid collection bottle 60;

[0064] Step 3): The temperature rises to a range below 10°C above the boiling point of methanol, distills methanol, and collects it in the heavy fraction liquid collection bottle 30;

[0065] Step 4): After the hydroxylation solution is cooled to 10°C, adjust the pH to 10 with...

Embodiment 2

[0073] Step 1): Add 2-methyl-5-nitroimidazole into the reaction kettle 20, add dropwise formic acid solvent with a concentration of 85% to dissolve 2-methyl-5-nitroimidazole, and add cyclic Oxyethane, add sulfuric acid with a concentration of 98% at the same time, raise the temperature to 85-95°C, and react for 1h to obtain a hydroxylated solution;

[0074] Step 2): close the reflux valve 51, open the outlet valve 71, add methanol, control the temperature within a range below 10°C higher than the boiling point of methyl formate, carry out esterification reaction, distill, and condense the steam that evaporates to obtain methyl formate , and collected by the light component liquid collection bottle 60;

[0075] Step 3): The temperature rises to a range below 10°C above the boiling point of methanol, distills methanol, and collects it in the heavy fraction liquid collection bottle 30;

[0076] Step 4): After the hydroxylation solution is cooled to 10°C, adjust the pH to 10 with...

Embodiment 3

[0084] Step 1): Add 2-methyl-5-nitroimidazole into the reaction kettle 20, add dropwise formic acid solvent with a concentration of 85% to dissolve 2-methyl-5-nitroimidazole, and add cyclic Oxyethane, add sulfuric acid with a concentration of 98% at the same time, raise the temperature to 85-95°C, and react for 1h to obtain a hydroxylated solution;

[0085] Step 2): close the reflux valve 51, open the outlet valve 71, add methanol, control the temperature within a range below 10°C higher than the boiling point of methyl formate, carry out esterification reaction, distill, and condense the steam that evaporates to obtain methyl formate , and collected by the light component liquid collection bottle 60;

[0086] Step 3): The temperature rises to a range below 10°C above the boiling point of methanol, distills methanol, and collects it in the heavy fraction liquid collection bottle 30;

[0087] Step 4): After the hydroxylation solution is cooled to 10°C, adjust the pH to 10 with...

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Abstract

The invention provides a method for applying formic acid glycol ester in metronidazole production, a device for achieving the method and a method for applying the device. According to the method for applying formic acid and glycol ester in metronidazole production, circulation application of formic acid glycol ester in the synthesis process of metronidazole is achieved, a part of formic acid is replaced by formic acid glycol ester, the application amount of formic acid can be reduced, and the production cost is saved. The device for achieving the method comprises a rectifying tower, a reactionkettle, a heavy component liquid collection bottle, a heavy component outlet pipe, a light component liquid collection bottle, a condenser and a light component outlet pipe. The device is simple in structure, convenient to use and high in practicability.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a method for applying ethylene glycol formate in the production of metronidazole, a device for realizing the method and a method for applying the device. Background technique [0002] Metronidazole is white or yellowish crystal or crystalline powder, used for the treatment of intestinal and parenteral amoebiasis (such as amebic liver abscess, pleural amoebiasis, etc.). It can also be used to treat vaginal trichomoniasis, cylindrosis, skin leishmaniasis, and guinea worm infection. At present, it is also widely used in the treatment of anaerobic infection, and is regarded as the drug of choice for anti-anaerobic bacteria by the World Health Organization (WHO). [0003] The current process of synthesizing metronidazole is to dissolve 2-methyl-5-nitroimidazole in formic acid, add ethylene oxide successively at 30-40°C, and add sulfuric acid in the middle of the addition. After addi...

Claims

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Application Information

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IPC IPC(8): C07D233/94
CPCC07D233/94
Inventor 曾舟华曾彩红刘晓晖冉敬文黄林勇杨水彬
Owner HUANGGANG NORMAL UNIV
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