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Process for preparing 2,6- dichlor-4-trifluoromethyl aniline

A technology of trifluoromethylaniline and trichlorobenzotrifluoride, which is applied in the field of preparation 2, can solve the problems of high reaction temperature and strong dependence on basic catalysts, achieve low reaction temperature, high reaction yield, and increase yield Effect

Active Publication Date: 2011-07-20
江西巍华化学有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The preparation method of Chinese patent polyhalogenated p-trifluoromethylaniline (patent No. CN 1330625A) discloses a kind of method for preparing 2,6-dichloro-4-trifluoromethylaniline, but there is a pair of basic catalysts in the reaction The problem of strong dependence and high reaction temperature

Method used

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  • Process for preparing 2,6- dichlor-4-trifluoromethyl aniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Preparation of 2,6-dichloro-4-trifluoromethylaniline:

[0021] Put 200g of 3,4,5-trichlorobenzotrifluoride and 145g of water into a 1000ml autoclave respectively, then close the reactor, fill it with 380g of liquid ammonia, close the valve after adding, turn on the stirring, and slowly raise the temperature to 160°C, the pressure rises to 10Mpa, and timed heat preservation is carried out. During the heat preservation period, the reaction temperature is controlled to 165°C, the pressure is 11.5Mpa, and the heat preservation time is 8h. After the heat preservation is completed, the pressure is released and the ammonia is discharged.

[0022] After the reaction material was washed with water, the reaction crude product was rectified, and 20.4 g of unreacted raw material 3,4,5-trichlorobenzotrifluoride was recovered to obtain 120 g of 2,6-dichloro-4-trifluoromethylaniline with a content of 99.24%. Yield 72.48%.

Embodiment 2- Embodiment 6

[0024] Device and operating steps are the same as in Example 1, and the results are shown in Table 1

[0025] Test results under different process conditions in table 1

[0026]

Embodiment 7

[0028] Put 200.0kg of 3,4,5-trichlorobenzotrifluoride, 130.0kg of water, and 360.0kg of liquid ammonia into a 1000L high-pressure reactor, close the reactor after feeding, start stirring, slowly raise the temperature to 170°C, and the initial pressure When the temperature is 0.2Mpa, start timing and heat preservation. During the heat preservation period, the reaction temperature is controlled at 170±5°C, the pressure is between 11.0-12.0Mpa, and the time is 9h. After the heat preservation is over, the material is cooled to 100°C, and the pressure in the primary absorption tank is controlled at Pressure relief and ammonia discharge between 0 and 1.8Mpa, and cooling with frozen brine. During the process of ammonia discharge, when the pressure in the primary absorption tank is greater than 1.8Mpa, it will enter the secondary absorption tank for absorption, during which the secondary absorption is controlled. The pressure in the tank is between 0 and 1.2Mpa. After the pressure reli...

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Abstract

The invention relates to a preparation method for 2, 6-dichloro-4-trifluromethylphenyl aniline, belonging to the technical field of organic chemistry. The starting materials of the invention are 3, 4, 5- trichloro benzotrifluoride and ammonia; wherein, the molar ratio of ammonia and 3, 4, 5- trichloro benzotrifluoride is 6 to 40:1; when the two materials react for one to thirty hours at the temperature of 150 DEG C to 178 DEG C and under the pressure of 1.0 MPa to 13.5 MPa, the product is separated to get 2, 6-dichloro-4-trifluromethylphenyl aniline and the excessive ammonia generated in the reaction is reclaimed. The method needs no catalysts or reaction solvent, keeps higher yield under the condition of lower reaction temperature; therefore, the method is characterized by simple technique and friendly environment, etc.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, relates to a method for preparing polyhalogenated aromatic amines, in particular provides a method for preparing 2,6-dichloro-4-trifluoromethylaniline. Background technique [0002] 2,6-dichloro-4-trifluoromethylaniline is an important pesticide intermediate used to prepare pyrazole compounds with insecticidal activity, such as the pyrazole insecticide "fipronil" (commodity known as Sharp). There are many preparation methods for 2,6-dichloro-4-trifluoromethylaniline. The general synthesis idea is to use 3,4-dichlorobenzotrifluoride as the raw material, which is first aminated and then halogenated. [0003] The preparation method of Chinese patent polyhalogenated p-trifluoromethylaniline (patent No. CN 1330625A) discloses a kind of method for preparing 2,6-dichloro-4-trifluoromethylaniline, but there is a pair of basic catalysts in the reaction Strong dependence and high reaction tempe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/52C07C209/10
Inventor 李惠跃陈静华吴江伟黄桂荣赵鑫平王凯泉
Owner 江西巍华化学有限公司