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Preparation method of bulk myclobutanil

A technology of myclobutanil and the original drug, applied in the field of preparation of myclobutanil original drug, can solve the problems of low purity, limited product yield, high production cost, etc.

Inactive Publication Date: 2009-09-23
HUBEI XIANLONG CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The present invention mainly solves technical problems such as complex production process, limited product yield, low purity and high production cost existing in the existing production process of myclobutanil technical

Method used

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  • Preparation method of bulk myclobutanil

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: the production of the original drug of myclobutanil mainly consists of the following steps:

[0017] One.1,2-(4-chlorophenyl) hexonitrile production: drop into p-chloronitrile benzyl, chlorinated n-butane, phase transfer catalyst tetrapropyl ammonium bromide successively in reactor (being chloronitrile benzyl weight 4 -6%, the same below), the temperature of the reactor is controlled at 55° C., and the mass concentration is slowly added dropwise to 50% sodium hydroxide solution, and the chlorinated benzyl: n-chlorobutane: the mol ratio of sodium hydroxide is controlled At 1: 1.2: 1.3, the dropping time is controlled at 3 hours. After the liquid caustic soda is dripped, the temperature is raised to 78°C to start timing and heat preservation. Wash with toluene and deionized water whose weight is 1 times the weight of n-chlorobutane, then let it stand and remove the lower wastewater in the reaction kettle, then feed in deionized water to wash the reaction pro...

Embodiment 2

[0020] Embodiment 2: the production of the original drug of myclobutanil mainly consists of the following steps:

[0021] One.1,2-(4-chlorophenyl) hexonitrile production: drop into p-chloronitrile benzyl, chlorinated n-butane, phase transfer catalyst tetrapropyl ammonium bromide successively in reactor (being chloronitrile benzyl weight 4 -6%, the same below), the reaction kettle temperature is controlled at 60 ℃, slowly dripping mass concentration is 50% sodium hydroxide solution, described p-chloronitrile benzyl: chlorobutane: the mol ratio control of sodium hydroxide At 1:1.4:1.5, the dropping time is controlled at 2 hours. After the liquid caustic soda is dripped, the temperature is raised to 77°C to start timing and heat preservation. Toluene and deionized water with a weight of 1.2 times the weight of n-chlorinated butane were washed, then left to stand and the lower layer of wastewater in the reactor was removed, and deionized water was added to wash the reaction produc...

Embodiment 3

[0024] Embodiment 3: the production of the original drug of myclobutanil mainly consists of the following steps:

[0025] -.1,2-(4-chlorophenyl) hexonitrile production: drop into p-chloronitrile benzyl, chlorinated n-butane, phase transfer catalyst tetrapropyl ammonium bromide successively in reactor (being chloronitrile benzyl weight 4 -6%, the same below), the reaction kettle temperature is controlled at 65 ℃, and slowly dripping mass concentration is 50% sodium hydroxide solution, and described p-chloronitrile benzyl: chlorobutane: the mol ratio control of sodium hydroxide At 1:1.6:1.7, the dropping time is controlled at 3 hours. After the drop of liquid caustic soda is completed, the temperature is raised to 75°C and the time insulation is started. Toluene and deionized water with a weight of 1.3 times the weight of n-chlorinated butane were washed, then left to stand and removed the lower wastewater in the reactor, and then fed into deionized water to wash the reaction pr...

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Abstract

The invention discloses a preparation method of bulk myclobutanil. A production method comprises the following steps: A, transferring p-chlorobenzonitrile, n-chlorobutane and tetrapropyl ammonium bromide into a reaction kettle, slowly adding a sodiumhydroxide solution with mass concentration of 50% dropwise to obtain 2-(4-chlorphenyl)hexanenitrile; B, sequentially transferring the 2-(4-chlorphenyl)hexanenitrile, dichloromethane and the tetrapropyl ammonium bromide into the reaction kettle, and slowly adding the sodiumhydroxide solution with mass concentration of 50% dropwise to obtain 1-chloro-2-nitrile-2-(4-chlorphenyl)hexane; and C, sequentially adding dimethyl sulphoxide, the sodiumhydroxide solution with mass concentration of 50% and 1,2,4-triazole to the reaction kettle to obtain a finished product of the bulk myclobutanil. Measurement shows that the bulk myclobutanil prepared by the preparation method has a white appearance and high purity above 98%.

Description

technical field [0001] The invention relates to the production field of myclobutanil, in particular to a preparation method of the original drug of myclobutanil. Background technique [0002] Myclobutanil is a triazole systemic fungicide, which is a white solid. Its structural formula is as follows: [0003] [0004] Myclobutanil has the characteristics of high efficiency, broad spectrum and low toxicity. It has good preventive and control effects on various diseases such as scab, black spot, and black spot. [0005] In the current production method of myclobutanil, the Chinese patent application No. 94111446.5 discloses a preparation method of the agricultural fungicide myclobutanil, although this method does not use expensive methylene bromide as a raw material, trying to reduce the production of myclobutanil. Cost of production. However, it is only suitable for small and medium-scale experiments. If this method is used to prepare the original drug of myclobutanil o...

Claims

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Application Information

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IPC IPC(8): C07D249/08A01N43/653A01P3/00
Inventor 范建国印常智刘志新张行
Owner HUBEI XIANLONG CHEM IND
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