Preparation method of metrafenone

A technology of metrafenone and chlorobenzene, applied in the field of organic synthetic chemistry, can solve problems such as low total yield, difficult purification and separation, and difficult industrial application

Inactive Publication Date: 2020-11-17
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method uses a graphite catalyst, and the yield of the product is improved a lot, but the total yield is still relatively low; it has more post-treatment steps during the reaction, and is also relatively complicated, and the purification and separation treatment is more difficult, and it is not easy to operate. It is more difficult to realize the industrialized application to test the proficiency of the on-site workers.

Method used

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  • Preparation method of metrafenone
  • Preparation method of metrafenone
  • Preparation method of metrafenone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0047] Embodiment: the concrete steps of the preparation method of a kind of metrafenone of the present invention are as follows:

[0048] (1) Diazotization reaction:

[0049] Depend on figure 1 As can be seen from the diazotization reaction process flow chart shown, the temperature of the mixed solution of 400kg of 42wt% sulfuric acid and 128.8kg of 2,3-dimethylaniline is lowered to -5~0°C, and then dropwise below the liquid surface Add 234.6kg of pre-prepared 30wt% sodium nitrite solution and stir well to obtain a diazo solution, which is stored below 0-5°C for direct use in the next step. Attention should be paid to the safety of diazotization in this step.

[0050] (2) Hydrolysis reaction:

[0051] Depend on figure 1 Shown hydrolysis reaction process flow sheet finds out, to the diazonium liquid of step 1 gained, add the sulfuric acid 534kg of boiling 42wt%, toluene 272kg and 2mmol quaternary ammonium salt phase-transfer catalyst (0.68kg tetrabutyl ammonium bromide) mi...

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Abstract

The invention discloses a preparation method of metrafenone, and belongs to the technical field of organic synthesis. The method comprises the following steps: respectively carrying out diazotizationreaction, hydrolysis reaction, etherification reaction, selective oxidation, positioning oxidation, bromination reaction, acylating chlorination reaction, bromination reaction, methylation reaction, methoxylation reaction and Friedel-Crafts acylation reaction to prepare a metrafenone (3'-bromo-2,3,4,6'-tetramethoxy-2',6-dimethyl benzophenone) product crude product; and refining to obtain the target product metrafenone. According to the method, the bottleneck problem in intermediate synthesis is solved, the metrafenone product is synthesized with low raw materials and production cost, and metrafenone with high purity and yield is obtained.

Description

Technical field: [0001] The invention belongs to the technical field of organic synthesis chemistry, and in particular relates to a benzophenone fungicide—metrafenone (3′-bromo-2,3,4,6′-tetramethoxy-2′,6-dimethyl The preparation method of base benzophenone). Background technique: [0002] Metrafenone is an important benzophenone fungicide, which is mainly used to control powdery mildew and eye spot disease of crops such as wheat and melons and fruits. It is also a dual-purpose fungicide for both prevention and treatment, and its mechanism of action Rather special. It was first developed by the American cyanamide company (BASF) in 1998. After being registered in Europe in 2004, it gradually began to be sold around the world, and soon had considerable economic benefits. So far, except for BASF Europe, which has been officially registered in China, no other company has been officially registered, and there are very few relevant materials reported on the total synthesis method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/46C07C49/84
CPCC07C45/46C07C41/16C07C37/62C07C51/60C07C51/363C07C51/29C07C45/28C07C245/06C07C37/045C07C49/84C07C43/2055C07C43/225C07C39/27C07C65/21C07C47/575C07C43/205C07C39/07
Inventor 苏丹张千峰张均贾爱铨
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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