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Synthesis method of 2-methylpyridine-N-oxide

A technology of picoline and synthesis method, which is applied in the field of pesticide/pharmaceutical chemical intermediates, can solve the problems of high preparation temperature, low product purity, and high water content, and achieve low water content, low discharge of three wastes, and production Safe and reliable effect

Active Publication Date: 2021-10-22
ANHUI XINGYU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Aiming at the problems of high preparation temperature, high pollution, low product purity and high water content of the existing 2-picoline-N-oxide, the present invention provides a synthesis method of 2-picoline-N-oxide, the raw material The conversion rate of 2-picoline can reach 99%, the product purity can reach 99%, and the moisture content is ≤0.5%.

Method used

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  • Synthesis method of 2-methylpyridine-N-oxide
  • Synthesis method of 2-methylpyridine-N-oxide
  • Synthesis method of 2-methylpyridine-N-oxide

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Embodiment 1

[0031] The 2-picoline-N-oxide compound synthesis method of the present embodiment uses benzene as a solvent, and uses molybdenum oxide and TEBA as a composite catalyst in the reaction process, comprising the following steps:

[0032] (1) Dissolving 2-picoline in benzene, the volume ratio of 2-picoline to benzene is 1:2 to obtain reaction solution A;

[0033] (2) Under low temperature conditions, slowly drop hydrogen peroxide into the reaction solution A, add excess hydrogen peroxide, and add molybdenum oxide and TEBA to react at the same time, the mass ratio of molybdenum oxide and TEBA is 1:3, the addition of the composite catalyst The amount is 3% of the total mass of raw materials; the follow-up reaction was carried out for 3 hours, so that the content of 2-picoline was controlled to be 0.5%, and the low temperature condition was 50°C; the mass fraction of hydrogen peroxide was 27.5%;

[0034] (3) After the reaction is completed, benzene is distilled under reduced pressure ...

Embodiment 2

[0047] The 2-picoline-N-oxide compound synthesis method of the present embodiment uses benzene as a solvent, and uses molybdenum oxide and TEBA as a composite catalyst in the reaction process, comprising the following steps:

[0048] (1) Dissolving 2-picoline in benzene, the volume ratio of 2-picoline to benzene is 1:2 to obtain reaction solution A;

[0049] (2) Under low temperature conditions, slowly drop hydrogen peroxide into the reaction solution A, add excess hydrogen peroxide, and add molybdenum oxide and TEBA to react at the same time, the mass ratio of molybdenum oxide and TEBA is 1:3, the addition of the composite catalyst The amount is 3.5% of the total mass of raw materials; the follow-up reaction was carried out for 3 hours, so that the content of 2-picoline was controlled to be 0.4%, and the low temperature condition was 50°C; the mass fraction of hydrogen peroxide was 27.5%;

[0050] (3) After the reaction is completed, benzene is distilled under reduced pressur...

Embodiment 3

[0063] The 2-picoline-N-oxide compound synthesis method of the present embodiment uses benzene as a solvent, and uses molybdenum oxide and TEBA as a composite catalyst in the reaction process, comprising the following steps:

[0064] (1) Dissolving 2-picoline in benzene, the volume ratio of 2-picoline to benzene is 1:2 to obtain reaction solution A;

[0065] (2) Under low temperature conditions, slowly drop hydrogen peroxide into the reaction solution A, add excess hydrogen peroxide, and add molybdenum oxide and TEBA to react at the same time, the mass ratio of molybdenum oxide and TEBA is 1:3, the addition of the composite catalyst The amount is 4% of the total mass of raw materials; the follow-up reaction was carried out for 4 hours, so that the content of 2-picoline was controlled to be 0.4%, and the described low temperature condition was 50°C; the mass fraction of hydrogen peroxide was 27.5%;

[0066] (3) After the reaction is completed, benzene is distilled under reduced...

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Abstract

The invention discloses a synthesis method of 2-methylpyridine-N-oxide, belonging to the technical field of pesticide / pharmaceutical chemical intermediates. According to the synthesis method, benzene is used as a solvent, and molybdenum oxide and TEBA are used as a composite catalyst in the reaction process. The synthesis method comprises the following steps: (1) dissolving 2-methylpyridine in benzene to obtain a reaction solution A; (2) slowly and dropwise adding hydrogen peroxide into the reaction solution A under a low-temperature condition of 50 DEG C, simultaneously adding molybdenum oxide and TEBA for a reaction, and tracking the reaction for 3-5 hours to control the content of 2-methylpyridine to be 0.5% or below; and (3) after the reaction is completed, distilling benzene under reduced pressure, and freezing the obtained reaction solution to obtain 2-methylpyridine-N-oxide. According to the method, benzene serves as the solvent, molybdenum oxide and TEBA serve as the composite catalyst, and hydrogen peroxide is slowly dropped, so side reactions are effectively controlled, and the purity of a product obtained after direct reaction reaches 99% or above.

Description

technical field [0001] The invention belongs to the technical field of pesticide / pharmaceutical chemical intermediates, and more specifically relates to a synthesis method of 2-picoline-N-oxide. Background technique [0002] Pyridine nitrogen oxides are an important class of organic chemical intermediates, which are widely used in pesticides, medicines, dyes, insecticides, synthetic resins, etc., especially in the application of new pesticides and medicines. The product of the regiment showed strong physiological activity. In particular, 2-picoline-N-oxide is an important drug intermediate for the new coronavirus, which requires high purity, acetic acid content ≤ 0.5%, and water content ≤ 0.5%. Due to the existence of the oxygen atom in the picoline nitrogen oxide, it can be used as an electron donor or an electron acceptor under different reaction conditions, so the nitrogen-oxygen group makes the 2 on the pyridine ring , The reactivity of nucleophilic substitution reacti...

Claims

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Application Information

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IPC IPC(8): C07D213/89
CPCC07D213/89Y02P20/584
Inventor 张升张宽宇万红根张太亮刘进水
Owner ANHUI XINGYU CHEM
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