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Continuous preparation method of 4-nitrosoantipyrine

A technology of nitrosoantipyrine and antipyrine, applied in chemical instruments and methods, organic chemistry, chemical/physical processes, etc., can solve the problem of increased reaction time by-products, many impurities in the product, and cumbersome purification process, etc. problems, to achieve the effect of easy processing, simple purification process and reduced purification cost

Active Publication Date: 2021-07-02
JIHENG PHARMA HENGSHUI CITY
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Problems solved by technology

[0005] The object of the present invention is to provide a kind of continuous preparation method of 4-nitroso antipyrine, in order to overcome above-mentioned antipyrine sulfate in the prior art Excessive nitrosation reaction time with sodium nitrite in the reactor leads to an increase in by-products, more impurities in the obtained product, more impurities in the subsequent production products, cumbersome subsequent purification process, and high purification costs

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  • Continuous preparation method of 4-nitrosoantipyrine
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  • Continuous preparation method of 4-nitrosoantipyrine

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preparation example Construction

[0045] The invention provides a continuous preparation method of 4-nitrosoantipyrine, the preparation method comprising the following steps:

[0046] Step S1, preparing an antipyrine sulfate solution.

[0047] Antipyrine and dilute sulfuric acid are added into a reaction kettle to prepare an antipyrine sulfate solution.

[0048] In a specific embodiment of the present invention, the mass concentration of the antipyrine sulfate solution prepared in step S1 is 30-40% (such as 31%, 32%, 33%, 34%, 35%, 36%, 37% , 38%, 39%).

[0049] Preferably, the mass concentration of the antipyrine sulfate solution prepared in step S1 is 32-36% (such as 33%, 34%, 35%).

[0050] Step S2, preparing an aqueous solution of sodium nitrite.

[0051] In a specific embodiment of the present invention, the mass concentration of the sodium nitrite aqueous solution prepared in step S2 is 15-20% (such as 16%, 17%, 18%, 19%).

[0052] Preferably, the mass concentration of the sodium nitrite aqueous soluti...

Embodiment 1

[0081] This embodiment provides a continuous preparation method of 4-nitrosoantipyrine, the preparation method comprising the following steps:

[0082] Step S1, preparation mass concentration is the antipyrine sulfate solution of 34%;

[0083] Step S2, preparing an aqueous sodium nitrite solution with a mass concentration of 18%;

[0084] Step S3, adding the antipyrine sulfate solution and sodium nitrite aqueous solution prepared in steps S1 and S2 respectively in the feed tank through the antipyrine sulfate feed inlet 11 and the sodium nitrite feed inlet, respectively Control the feeding rate of antipyrine sulfate solution to be 1.35m 3 / h, the feed rate of sodium nitrite aqueous solution is 1.4m 3 / h, the temperature of reaction in the control feed tank is 50 DEG C, and the stirring speed of the first stirring device 2 is 218rpm, obtains semi-finished product 4-nitrosoantipyrine;

[0085] The semi-finished product 4-nitrosoantipyrine obtained in step S4 and step S3 enters...

Embodiment 2

[0088] This embodiment provides a continuous preparation method of 4-nitrosoantipyrine, the preparation method comprising the following steps:

[0089] Step S1, preparation mass concentration is the antipyrine sulfate solution of 32%;

[0090] Step S2, preparing an aqueous sodium nitrite solution with a mass concentration of 18%;

[0091] Step S3, adding the antipyrine sulfate solution and sodium nitrite aqueous solution prepared in steps S1 and S2 respectively in the feed tank through the antipyrine sulfate feed inlet 11 and the sodium nitrite feed inlet, respectively Control the feeding rate of antipyrine sulfate solution to be 1.2m 3 / h, the feed rate of sodium nitrite aqueous solution is 1.2m 3 / h, the temperature of reaction in the control feed tank is 50 DEG C, and the stirring speed of the first stirring device 2 is 220rpm, obtains semi-finished product 4-nitrosoantipyrine;

[0092] The semi-finished product 4-nitrosoantipyrine obtained in step S4 and step S3 enters ...

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Abstract

The invention provides a continuous preparation method of 4-nitrosoantipyrine. The continuous preparation method comprises the following steps: step S1, preparing an antipyrine sulfate solution; S2, preparing a sodium nitrite aqueous solution; S3, respectively adding the antipyrine sulfate solution and the sodium nitrite aqueous solution into a feeding tank, controlling the temperature in the feeding tank, and reacting the two materials to obtain a semi-finished product 4-nitrosoantipyrine; and S4, feeding the semi-finished product 4-nitrosoantipyrine into a discharging tank through a connecting pipe, controlling the temperature of the discharging tank, conducting stirring for reaction, and enabling the product to flow out through a discharging port, so as to obtain the finished product 4-nitrosoantipyrine. According to the method, feeding and discharging are carried out at the same time, continuous generation of the 4-nitrosoantipyrine is achieved, the situation that the reaction time is too long or the reaction is insufficient can be well avoided, the prepared 4-nitrosoantipyrine is high in yield and low in impurity content, the subsequent purification process is simple, and the purification cost is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of synthesis of analgin intermediates, and in particular relates to a continuous preparation method of 4-nitrosoantipyrine. Background technique [0002] Analgin (Metamizole Sodium Tablets), a compound that combines aminopyrine and sodium sulfite, is easily soluble in water, and has faster and stronger antipyretic and analgesic effects than aminopyrine. 4-Nitrosoantipyrine is a synthetic analgin It is an important intermediate. In the prior art, antipyrine sulfate solution and sodium nitrite solution are added into a batch reaction kettle through nitrosation reaction to obtain 4-nitrosoantipyrine. [0003] But because the reduction reaction of antipyrine sulfate and sodium nitrite is fast, the too long reaction time can cause the increase of by-product, make the content of 4-nitroso antipyrine relatively low (can only reach 85%), if If the reaction time is too short, part of the reactants will not be able t...

Claims

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Application Information

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IPC IPC(8): B01J19/18B01J19/00B01J4/00C07D231/52
CPCB01J19/18B01J19/0066B01J4/001C07D231/52
Inventor 马胜义魏蒙蒙徐亚威魏晶磊刘晓莲王光强蔡世恒商文雨王健孙若飞代国爱焦银蕾段广播
Owner JIHENG PHARMA HENGSHUI CITY
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