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Preparation method of isoniazid

A technology of isoniazid and isonicotinic acid, applied in organic chemistry and other directions, can solve problems such as difficult operability and controllability, narrow temperature range, etc., and achieves wide reaction temperature range, improved yield and quality, and large selection. range effect

Active Publication Date: 2021-04-30
GUANGZHOU BAIYUNSHAN MINGXING PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the problems of narrow temperature range limitation, operability and controllability of the existing isoniazid synthesis method, and to provide a new isoniazid preparation method

Method used

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  • Preparation method of isoniazid
  • Preparation method of isoniazid
  • Preparation method of isoniazid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Embodiment 1 A kind of preparation of isoniazid

[0053] S1, the synthesis of isoniazid

[0054] Dissolve 150kg of isonicotinic acid in 258kg of 40% hydrazine hydrate, distill under reduced pressure to 79-82°C, then change to normal pressure environment, rapidly raise the temperature of the reaction system to 129°C, react for 3 hours, add 193.5kg of purified water to quench The reaction was carried out to obtain the crude product suspension of isoniazid.

[0055] S2, refining of isoniazid

[0056] S2-1. Decolorization: Cool the crude isoniazid suspension obtained in the above step S1. at room temperature for 4 hours, heat the cooled crude suspension to 70-80°C to dissolve, add 2% activated carbon, and stir for 15 minutes. Filter while hot with a filter cloth with a mesh number of 325, quickly transfer the filtrate to the crystallization kettle, gradually cool down and crystallize until the system temperature is 5-10°C, control the cooling and crystallization time for ...

Embodiment 7

[0070] Embodiment 7 A kind of preparation of isoniazid

[0071] S1, the synthesis of isoniazid

[0072] Dissolve 150kg of isonicotinic acid in 258kg of 40% hydrazine hydrate, distill under reduced pressure to 79-82°C, then change to normal pressure environment, rapidly raise the temperature of the reaction system to 135°C, react for 3 hours, add 223.5kg of purified water to quench The reaction was carried out to obtain the crude product suspension of isoniazid.

[0073] S2, refining of isoniazid

[0074] S2-1. Decolorization: Cool the crude isoniazid suspension obtained in the above step S1. at room temperature for 4 hours, heat the cooled crude suspension to 70-80°C to dissolve, add 2% activated carbon, and stir for 15 minutes. Filter while hot with a filter cloth with a mesh number of 325, quickly transfer the filtrate to the crystallization kettle, gradually cool down and crystallize until the system temperature is 5-10°C, control the cooling and crystallization time for ...

Embodiment 8

[0084] Embodiment 8 A kind of preparation of isoniazid

[0085] S1, the synthesis of isoniazid

[0086] Dissolve 150kg of isonicotinic acid in 258kg of 40% hydrazine hydrate, distill under reduced pressure to 79-82°C, then change to normal pressure environment, rapidly raise the temperature of the reaction system to 135°C, react for 3 hours, add 193.5kg of purified water to quench The reaction was carried out to obtain the crude product suspension of isoniazid.

[0087] S2, refining of isoniazid

[0088] S2-1. Decolorization: Cool the crude isoniazid suspension obtained in the above step S1. at room temperature for 4 hours, heat the cooled crude suspension to 70-80°C to dissolve, add 2% activated carbon, and stir for 15 minutes. Filter while hot with a filter cloth with a mesh number of 325, quickly transfer the filtrate to the crystallization kettle, gradually cool down and crystallize until the system temperature is 5-10°C, control the cooling and crystallization time for ...

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Abstract

The invention discloses a preparation method of isoniazide, which adopts temperature control and proper increase of hydrazine hydrate feeding proportion for reaction, solves the problems of narrow temperature range and difficult operability and controllability of the traditional condensation reaction, widens the reaction temperature to 129-138 DEG C, and has high yield of isoniazide. Meanwhile, refining steps such as decoloration, washing and recrystallization are combined, so that the content of impurities in isoniazid is remarkably reduced, and the requirements of related evaluation work of crude drugs are met. The reaction temperature range is wide, the yield and purity of isoniazide are improved, and a larger selection range is provided for operability and controllability of industrial production of isoniazide.

Description

technical field [0001] The invention belongs to the technical field of isoniazid preparation. More specifically, it relates to a preparation method of isoniazid. Background technique [0002] Isoniazid (Isoniazid) chemical name: 4-pyridinyl hydrazide, and rifampicin, ethambutol and pyrazinamide are the first-line anti-tuberculosis drugs. As a chemical drug, isoniazid was invented in 1952. The invention of isoniazid has brought about fundamental changes in the treatment of tuberculosis. Drug resistance, but most doctors still believe that it is an indispensable main drug for the treatment of tuberculosis. [0003] At present, there are mainly two methods for the synthesis of isoniazid: the first is to use 4-cyanopyridine as a raw material, hydrolyze it into isonicotinamide, and then condense it with pure hydrazine (Sycheva TP, Pavlova TN, Shehukina MN. Synthesis ofisoniazid from 4-cyanopyridine.Pharma Chem J,1972:6:696-698.), the shortcoming of this synthetic route is that...

Claims

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Application Information

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IPC IPC(8): C07D213/86
CPCC07D213/86
Inventor 刘宏李同根黄晓丹黄子健李心花卢瑞芯黄孟秋陈思园
Owner GUANGZHOU BAIYUNSHAN MINGXING PHARM CO LTD
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