A kind of synthetic method of methylpiperium former medicine

A synthesis method and mepinium technology are applied in the field of synthesis of mepinium original medicine, and achieve the effects of high purity, simple process operation, significant economic benefits and social benefits

Active Publication Date: 2019-03-22
ANYANG XIAOKANG PESTICIDE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved in the present invention is: aiming at the technical problems existing in the existing mepiperium synthesis method, the present invention provides a method for synthesizing high-purity mepiperium using pyridine as a raw material

Method used

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  • A kind of synthetic method of methylpiperium former medicine
  • A kind of synthetic method of methylpiperium former medicine
  • A kind of synthetic method of methylpiperium former medicine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The synthetic method of the former medicine of methylpiperium of the present invention, the detailed steps of this synthetic method are as follows:

[0039] a. First, add ethanol with a mass percentage concentration of 99.5% into the reaction vessel, then add the raw material pyridine for mixing, and add methyl chloride after dissolving; then heat up to 80°C, and control the pressure during the reaction to 0.5MPa. 1. Reaction under pressure conditions for 6h, and N-picoline chloride was obtained after the reaction;

[0040] The mass ratio of the amount added between the pyridine and ethanol is 1:2.5; the molar ratio of the amount added between the pyridine and methyl chloride is 1:1.2;

[0041] B, adding the N-picoline chloride obtained in step a and the bimetallic supported catalyst Ru-Pd / C in the reaction vessel, the addition of the catalyst accounts for 4% of the N-picoline chloride quality; then Pass hydrogen into the reactor, the molar ratio between the N-picoline...

Embodiment 2

[0047] The synthetic method of the former medicine of methylpiperium of the present invention, the detailed steps of this synthetic method are as follows:

[0048] a. First, add ethanol with a mass percentage concentration of 97% into the reaction vessel, then add the raw material pyridine for mixing, and add methyl chloride after dissolving; then heat up to 100°C, and control the pressure during the reaction to 0.7MPa. 1. Reaction under pressure conditions for 4h, and N-picoline chloride was obtained after the reaction;

[0049]The mass ratio of the amount added between the pyridine and ethanol is 1:3.5; the molar ratio of the amount added between the pyridine and methyl chloride is 1:1.1;

[0050] B, the N-picoline chloride that step a obtains and PTP-20 pyridine hydrogenation catalyst are added in the reaction vessel, the addition of described catalyst accounts for 3% of N-picoline chloride quality; Then to reactor Introduce hydrogen gas, the molar ratio between the N-pico...

Embodiment 3

[0056] The synthetic method of the former medicine of methylpiperium of the present invention, the detailed steps of this synthetic method are as follows:

[0057] a. First, add ethanol with a mass percentage concentration of 95% into the reaction vessel, then add the raw material pyridine for mixing, and add methyl chloride after dissolving; then heat up to 60°C, and control the pressure during the reaction to 0.9MPa. 1. Reaction under pressure conditions for 6h, and N-picoline chloride was obtained after the reaction;

[0058] The mass ratio of the amount added between the pyridine and ethanol is 1:5; the molar ratio of the amount added between the pyridine and methyl chloride is 1:1.2;

[0059] B, adding the N-picoline chloride obtained in step a and the bimetallic supported catalyst Ru-Pd / C into the reaction vessel, the addition of the catalyst accounts for 5% of the N-picoline chloride quality; then Pass hydrogen into the reactor, the molar ratio between the N-picoline c...

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Abstract

The invention discloses a method for synthesizing a mepiquat chloride original medicine. The method comprises the following steps: adding ethanol into a container, adding pyridine for mixing, adding chloromethane after dissolution, and performing heating reaction to obtain N-methylpyridine chloride; adding the N-methylpyridine chloride and a catalyst into a reaction container, introducing hydrogen, performing heating reaction to obtain an N-methylpiperidine hydrochloride system, adding an acid binding agent into the N-methylpiperidine hydrochloride system for neutralization reaction, and performing filtering to obtain N-methylpiperidine; dissolving the N-methylpiperidine in ethanol, and adding chloromethane for heating reaction; evaporating a reaction system to remove the ethanol and the chloromethane to obtain a high-purity mepiquat chloride product. According to the method, the using amount of the acid binding agent is reduced in a production process, and the water cost for production is reduced; in addition, the sustainability is high, the energy consumption is effectively reduced, and the method is a novel production process. Therefore, the method has remarkable economic benefits and social benefits.

Description

1. Technical field: [0001] The invention relates to the technical field of medicine synthesis technology, in particular to a method for synthesizing the original drug of mepiperium. 2. Background technology: [0002] Methylpiperium is a new type of plant growth regulator, which has a good systemic conduction effect on plants; Methylpiperium can promote the reproductive growth of plants, inhibit the growth of stems and leaves, control side branches, shape ideal plant shapes, and increase the number and vitality of roots; And it can increase the weight and quality of the fruit. Methylpiperium is widely used in crops such as cotton, wheat, rice, peanuts, corn, potatoes, grapes, vegetables, beans and flowers. Methylpiperium is a systemic drug with high efficiency, low toxicity and no harm. Spraying methylpiperium according to the dosage and different growth stages of plants can regulate plant growth, make plants firm and resistant to lodging, improve color and increase yield. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/037C07D295/023
CPCC07D295/023C07D295/037
Inventor 张继昌张黎明刘小涛王晶晶李帅刘永娜
Owner ANYANG XIAOKANG PESTICIDE
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