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Synthesis method for 2, 4-dichloro-5-isopropoxyaniline

A technology of propoxyaniline and synthesis method, which is applied in two fields, can solve the problems such as difficult recovery of catalyst, difficult recovery of catalyst, easy poisoning of catalyst, etc., and achieve great economic benefits and industrial application prospects, easy control of reaction, and effects of not easy poisoning

Inactive Publication Date: 2019-02-15
ANHUI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Hydrazine hydrate reduction is prone to produce a large amount of waste acid and waste water, and the catalyst is difficult to recover. Although hydrogenation reduction has the advantages of easy control, high product purity, high yield, less waste, and fast reaction rate, it also has the advantages of using precious metal catalysts. Defects such as high cost, easy poisoning of the catalyst, easy spontaneous combustion of the catalyst, and difficult recycling of the catalyst

Method used

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  • Synthesis method for 2, 4-dichloro-5-isopropoxyaniline

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preparation example Construction

[0020] The invention discloses a synthesis method of 2,4-dichloro-5-isopropoxyaniline, specifically discloses a synthesis method of 2,4-dichloro-5-isopropoxyaniline, comprising the following steps:

[0021] S1. Putting auxiliary agents and catalysts into the reactor to obtain the first mixed solution;

[0022] S2. Putting an organic solvent and a raw material compound into the first mixed liquid, and feeding hydrogen gas into the reaction vessel, so that the original compound undergoes a reduction reaction with the hydrogen gas in the presence of an organic solvent, an auxiliary agent and a catalyst, And obtain the reaction product;

[0023] S3. Remove the catalyst and solvent from the reaction product to obtain 2,4-dichloro-5-isopropoxyaniline.

[0024] Wherein, the catalyst is a nano-catalyst, such as a nano-nickel catalyst.

[0025] Overall chemical reaction equation of the present invention is as follows:

[0026]

Embodiment 1

[0028] The invention discloses a synthesis method of 2,4-dichloro-5-isopropoxyaniline, comprising the following steps:

[0029] S1. Add 4-6g of nano-catalyst with a particle size of 90-100nm and 48-53ml of adjuvant into a reaction kettle with a capacity of 1-2L, and start stirring to fully mix the two.

[0030] S2. After waiting for stirring for 20 to 30 minutes, add 392 to 400 ml of toluene and 247 to 251 g of 2,4-dichloro-5-isopropoxyaniline into the reaction kettle;

[0031] S3. Introduce nitrogen into the reactor to replace the air in the reactor, and then turn off the introduction of nitrogen after 8 to 10 minutes, and then inject hydrogen into the reactor to replace the nitrogen in the reactor , after another 8 to 10 minutes, turn off the introduction of hydrogen, and then feed nitrogen into the reaction kettle again to replace the hydrogen. After repeating three times, keep the hydrogen pressure in the reaction kettle at 2 to 3 MPa, raise the temperature to 98 to 104 ° ...

Embodiment 2

[0035] The invention discloses a synthesis method of 2,4-dichloro-5-isopropoxyaniline, comprising the following steps:

[0036] S1. Add 1.6-2.5g of nano-catalysts with a particle size of 10-20nm and 15-20ml of adjuvants into a reaction kettle with a capacity of 1-2L, and start stirring to fully mix the two. ;

[0037] S2. After waiting for stirring for 20 to 30 minutes, add 200 to 210 ml of dichloroethane and 247 to 251 g of 2,4-dichloro-5-isopropoxyaniline into the reaction kettle;

[0038] S3. Introduce nitrogen into the reactor to replace the air in the reactor, and then turn off the introduction of nitrogen after 8 to 10 minutes, and then inject hydrogen into the reactor to replace the nitrogen in the reactor , after another 8 to 10 minutes, turn off the introduction of hydrogen, and then feed nitrogen into the reactor again to replace the hydrogen. After repeating three times, keep the hydrogen pressure in the reactor at 4 to 5 MPa, raise the temperature to 75 to 85°C, a...

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Abstract

The invention discloses a synthesis method for 2, 4-dichloro-5-isopropoxyaniline. The method comprises the following steps: feeding an auxiliary agent and a catalyst into a reaction kettle, so as to obtain first mixed liquor; feeding an organic solvent and an original compound into the first mixed liquor, and feeding hydrogen into the reaction kettle, so as to ensure that the original compound performs reduction reaction in the condition of the existence of the organic solvent, the auxiliary agent and the catalyst and obtain a reaction product; removing the catalyst and solvent of the reactionproduct, so as to obtain the 2, 4-dichloro-5-isopropoxyaniline. The catalyst adopts a nano-catalyst. The method simplifies synthesis steps of the 2, 4-dichloro-5-isopropoxyaniline, reduces the cost and the recycling difficulty of the catalyst, and meanwhile avoids ricks in traditional technical processes.

Description

technical field [0001] The invention relates to a production process of oxadiazone, in particular to a synthesis method of 2,4-dichloro-5-isopropoxyaniline. Background technique [0002] Oxadiazon is a nitrogen-containing heterocyclic herbicide developed by the French company Rhone-Polanck. The drug has low toxicity, good ecological benefits, safety to crops, convenient use, and wide application of crops, such as rice, peanuts, cotton and other water and dry crops. Its chemical name is: 5-tert-butyl-3-(2,4-dichloro-5-isopropoxyphenyl)-1,3,4-oxadiazolin-2-one. [0003] At present, there are two processes for preparing 2,4-dichloro-5-isopropoxyaniline, which are hydrazine hydrate reduction and hydrogenation reduction. Hydrazine hydrate reduction is prone to produce a large amount of waste acid and waste water, and the catalyst is difficult to recover. Although hydrogenation reduction has the advantages of easy control, high product purity, high yield, less waste, and fast re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/76C07C213/02
CPCC07C213/02C07C215/76Y02P20/584
Inventor 李牣房希婷徐守明
Owner ANHUI RES INST OF CHEM IND
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