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Novel synthesis method of mequindox

A technique for the synthesis of acemethaquine, which is applied in the field of organic chemical synthesis, can solve problems such as slow reaction speed, difficulty in control, and strong activity of soda ash, and achieve the effects of easy control of the reaction, shortened reaction time, and improved catalytic efficiency

Inactive Publication Date: 2019-10-11
浙江科泓企业管理咨询有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Soda ash or anhydrous sodium acetate are adopted in the existing acetylmethaquine synthetic process, and soda ash and anhydrous sodium acetate are all insoluble in ethanol and methanol, and the reaction speed is relatively slow, and after

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0016] A novel synthetic method of methequine, including the following steps:

[0017] (1) Weigh benzoxadiazepine-N-oxide and organic solvent into the reactor, start stirring, and heat to 55°C,

[0018] (2) Weigh acetylacetone and add it to the reaction kettle, and keep the temperature at 55~62℃ for 2 hours.

[0019] (3) Add the weighed potassium acetate in multiple times, keep the temperature at 60~65℃ for 2~3 hours, cool to 20~25℃, separate with a centrifuge, wash the filter cake with organic solvent, and dry to obtain methyl acetyl. Crude quinine.

[0020] Preferably, the organic solvent is methanol or ethanol.

[0021] Preferably, acetylacetone: benzoxadiazepine-N-oxide: organic solvent: potassium acetate=11.5:16.5:15:5.5.

[0022] Preferably, potassium acetate is added to the reaction kettle in five times, with the same amount each time.

[0023] Preferably, potassium acetate is potassium acetate powder.

[0024] Preferably, the drying adopts a centrifuge spin drying or a filter pres...

Example Embodiment

[0025] Example 1: A new method for synthesizing methaquine, including the following steps:

[0026] (1) Weigh 1650 grams of benzoxadiazepine-N-oxide and 1500 grams of ethanol into the reactor, start stirring, and heat to 55°C.

[0027] (2) Weigh 1150 grams of acetylacetone into the reaction kettle, and keep the temperature at 55~62℃ for 2 hours.

[0028] (3) Add 55 grams of potassium acetate weighed in 5 times, add 11 grams of potassium acetate at a time, keep the reaction at 60~65℃ for 2~3 hours, cool to 20~25℃, separate with centrifuge, and filter cake with organic The solvent is cleaned, and the crude methequine is obtained after centrifugal drying in a centrifuge.

Example Embodiment

[0029] Example two, a novel method for synthesizing methequine, including the following steps:

[0030] (1) Weigh 1650 grams of benzoxadiazepine-N-oxide and 1500 grams of methanol into the reactor, start stirring, and heat to 55°C.

[0031] (2) Weigh 1150 grams of acetylacetone into the reaction kettle, and keep the temperature at 55~62℃ for 2 hours.

[0032] (3) Add 55 grams of potassium acetate weighed in 5 times, add 11 grams of potassium acetate at a time, keep the reaction at 60~65℃ for 2~3 hours, cool to 20~25℃, separate with centrifuge, and filter cake with organic The solvent is washed, and the crude methequine is obtained after pressure filtration and drying with a filter press.

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PUM

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Abstract

The invention relates to a novel synthesis method of mequindox. The method comprises the following steps of 1, weighing benzo oxazo dinitrogen pentyl-N-oxide and an organic solvent, putting the materials in a reaction kettle, starting to stir the materials, and then heating the reaction kettle to 55 DEG C; 2, weighing acetylacetone, adding the acetylacetone in the reaction kettle, controlling thetemperature to be 55-62 DEG C, and then maintaining the temperature for 2 hours; 3, adding weighed potassium acetate repeatedly, maintaining the temperature of 60-65 DEG C for 2-3 hours of a reaction,then decreasing the temperature to 20-25 DEG C, utilizing a centrifugal machine for separation, cleaning filter cakes with an organic solvent, and then drying to obtain a crude product of mequindox.The method has the advantages that the potassium acetate is adopted as a catalyst, since the potassium acetate is dissolved quickly in methyl alcohol or ethyl alcohol, the catalysis efficiency is improved, the alkalinity of the potassium acetate is weaker than that of sodium carbonate, and the reaction is easy to control; as is indicated by experimental data, when the potassium acetate is selectedas the catalyst, the yield of the product is increased by 13%, and the reaction time is shortened to 2-3 hours.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a novel synthesis method of acemethaquine. Background technique [0002] Soda ash or anhydrous sodium acetate are adopted in the existing acetylmethaquine synthetic process, and soda ash and anhydrous sodium acetate are all insoluble in ethanol and methanol, and the reaction speed is relatively slow, and after soda ash dissolves, the activity is too strong, it is difficult to control, and it is easy to produce The side reaction has a great impact on the recovery rate of acemethaquine, so a new catalyst is needed to replace soda ash or anhydrous sodium acetate. Contents of the invention [0003] The purpose of the present invention is to overcome the above problems that the prior art exists, and a kind of novel synthetic method of acetylmethaquine is provided, adopts potassium acetate to make catalyzer, has improved catalytic efficiency. [0004] In order to achieve th...

Claims

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Application Information

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IPC IPC(8): C07D241/52
CPCC07D241/52
Inventor 姚凯
Owner 浙江科泓企业管理咨询有限公司
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