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Novel technique for preparing 4-formyl amino antipyrine

A technology of aminoantipyrine and antipyrine, applied in the direction of organic chemistry, can solve the problems of incomplete separation of feed liquid and colloid, high cost of production raw materials, and affecting the quality of finished products, and achieve large-scale continuous automatic operation , easy to extract and stratify, and reduce the workload

Active Publication Date: 2009-02-04
SHANDONG XINHUA PHARMA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This treatment method is a physical separation method, the separation of the feed liquid and the colloid is not complete, the colloid contains the material, and the feed liquid also contains the remaining colloid, which seriously affects the quality of the intermediate in the subsequent process and the quality of the finished product, and wastes a lot of materials.
At the same time, this treatment method has a long process flow, cumbersome operation, low production efficiency, high energy consumption, and high raw material cost.

Method used

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  • Novel technique for preparing 4-formyl amino antipyrine

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Embodiment Construction

[0020] The present invention does not change the original production conditions of each reaction step (nitrosation, reduction, hydrolysis, neutralization, acylation).

[0021] Take 800ml of 4-aminoantipyrine hydrolyzate (the mass content of 4-aminoantipyrine is about 12%), cool down to 55°C, add chloroform to extract according to a certain volume ratio of hydrolyzate and chloroform, and the extraction temperature is 45-55°C. ℃. During the extraction process, the chloroform layer containing the colloid in the lower layer is separated, the chloroform is recovered by distillation, and the chloroform is recycled. Take the hydrolyzed solution in the upper layer according to the original process, neutralize and acylate to obtain 4-formylaminoantipyrine.

[0022] Add chloroform extraction with hydrolyzate and chloroform certain volume ratio (1: 1, 1: 0.5, 1: 0.3) below, compare with the original process, the result is as follows:

[0023]

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Abstract

The invention provides a new technique for preparing intermediate 4-formyl amino antipyrine. Antipyrine carries out a plurality of technique steps, including nitrosation, reduction, hydrolysis, neutralization and acylation. The new technique is characterized in that: 4-formyl amino antipyrine hydrolysate which is obtained after the nitrosation, reduction and hydrolysis carries out colloid treatment, neutralization and acylation reaction to prepare 4-formyl amino antipyrine. The colloid impurity treatment includes the steps: extractant is added into 4-amino antipyrine hydrolysate, and colloid impurity is removed after extracting. The new technique for preparing 4-formyl amino antipyrine hydrolysate improves the quality of analgin intermediate greatly, reduces the labor intensity and production cost greatly, simplifies production technical process, improves production efficiency, saves energy and reduces consumption, saves workshop equipment, and brings considerable economic benefit for the enterprises.

Description

technical field [0001] The invention relates to a chemical synthesis preparation process, in particular to a preparation process of analgin intermediate 4-formylaminoantipyrine, an antipyretic and analgesic drug. Background technique [0002] Analgin is mainly used for reducing fever, and is also used to treat acute arthritis, headache, rheumatic pain, toothache and muscle pain, etc. [0003] The synthesis of Analgin uses pyrazolone as the starting material to produce antipyrine, which then produces 4-aminoantipyrine, and 4-aminoantipyrine then produces 4-formyl Aminoantipyrine and 4-formylaminoantipyrine are then produced into 4-methylaminoantipyrine, and 4-methylaminoantipyrine is condensed to produce the finished product Analgin. [0004] Wherein 4-formylaminoantipyrine is one of the important intermediates of synthetic Sulpyrine, but due to the process of synthesizing Sulpyrine intermediate antipyrine and 4-aminoantipyrine, it needs to go through high temperature And p...

Claims

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Application Information

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IPC IPC(8): C07D231/50
Inventor 杨成顺王凯广徐明卢维刚王均华
Owner SHANDONG XINHUA PHARMA CO LTD
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