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Synthesis method of 5-chlorine-2-phenoxyaniline and Beta molecular sieve used in synthesis method

A technology of phenoxyaniline and synthesis method, which is applied in the direction of molecular sieve catalysts, preparation of amino compounds, chemical instruments and methods, etc., can solve problems such as high reaction temperature and complex design of rectification tower, so as to achieve no waste generation and energy saving Effect

Active Publication Date: 2018-12-14
JINHUA SHUANGHONG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are obvious defects in this process: firstly, the reaction temperature is relatively high, generally at 160-180°C, and a variety of non-target products are generated during the process, such as reacting with solvents, producing coke, etc.; secondly, the reaction products must be separated, To separate water and solvent from the product, and then separate a large number of by-products in the product, this process requires solvent extraction or vacuum distillation, and the design of the rectification column often becomes different due to the different properties of the material. complex
Reduction catalyst involved in the present invention---the preparation and use of Beta molecular sieve reduction catalyst have not been reported yet

Method used

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  • Synthesis method of 5-chlorine-2-phenoxyaniline and Beta molecular sieve used in synthesis method
  • Synthesis method of 5-chlorine-2-phenoxyaniline and Beta molecular sieve used in synthesis method
  • Synthesis method of 5-chlorine-2-phenoxyaniline and Beta molecular sieve used in synthesis method

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0050] The preparation of example 1, a kind of Beta molecular sieve reduction catalyst, carries out following steps successively:

[0051] The following parts refer to parts by mass.

[0052] ①, 2.05 parts of NaAlO 2 (content in Al 2 o 3 ≥ 41.0%), 0.5 parts of NaOH (≥ 98%), 20.4 parts of water and 14.7 parts of tetraethylammonium hydroxide aqueous solution (tetraethylammonium hydroxide mass concentration is 25%) mixed, after stirring at 20 ° C for 20min, Add 22.5 parts of silica gel therein, and continue stirring for 30 minutes to obtain a gel mixture.

[0053] Silica gel can be selected from the chromatography silica gel H (200-300 mesh) of Qingdao Ocean Chemical Co., Ltd.

[0054] Move the gel mixture into a stainless steel synthesis kettle and seal it. After crystallization at 80°C for 10h, raise the temperature to 130°C, crystallize for 20h, cool to room temperature, wash 10 parts with deionized water, filter out water, and dry at 130°C 4h, and then calcined in a muff...

Embodiment 1

[0058] Embodiment 1, a kind of preparation method of 5-chloro-2-phenoxyaniline, carries out following steps successively:

[0059]

[0060] 1), 192.0g (1.0mol) 2,5-dichloronitrobenzene, heated up to 100°C, melted and stirred for 30 minutes, added 3.84g of condensation phase transfer catalyst APG, then alternately added 63g of sodium hydroxide and 103.0g of phenol (divided into 5 alternate additions), heated to 125°C after the addition, and kept stirring for 240 minutes;

[0061] 2), the reaction product obtained in step 1) is cooled to 60°C, slowly add 400g water, 600g 80% (volume %) ethanol aqueous solution, add 95g 85% hydrazine hydrate (1.6mol), add 2.5g Beta molecular sieve reduction Catalyst, heated to reflux, reflux reaction for 220 minutes, reduction reaction to the end, cooling to 40 ° C, filtering out the Beta molecular sieve catalyst, adding 500 g of water to the filtrate, heating up to distill ethanol, when the distillation temperature rose to 96 ° C, stop heatin...

Embodiment 2

[0062] Embodiment 2, "600g80% (volume %) ethanol aqueous solution " in the replacement embodiment 1 of reclaiming ethanol (80%, volume %) 600g of embodiment 1 gained, all the other are equal to embodiment 1. Finally, 213.5 g (100%) of 5-chloro-2-phenoxyaniline was obtained, with a yield of 97.6% and a purity of 98%.

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Abstract

The invention discloses a synthesis method of 5-chlorine-2-phenoxyaniline. The synthesis method comprises the following steps: 1) heating 2, 5-dichloronitrobenzene to be melted in a solvent-free state, adding a condensation phase transfer catalyst into the melted 2, 5-dichloronitrobenzene, then adding sodium hydroxide and phenol into the mixture and performing a reaction at the temperature of 60-130 DEG C for 3-5h; 2) cooling a reaction product, adding a solvent, hydrazine hydrate and a Beta molecular sieve reduction catalyst into the reaction product, heating the mixture to backflow and performing a reduction reaction; 3) after a backflow reaction in step 2) is ended, performing filtration to obtain the Beta molecular sieve reduction catalyst and filtrate, distilling the filtrate to obtain alcohol in the solvent, cooling to 15-20 DEG C, stirring the mixture for 3-5h, performing separation by crystallization and performing filtration, so as to obtain the 5-chlorine-2-phenoxyaniline asa filter cake. The 5-chlorine-2-phenoxyaniline is synthesized by adopting the method disclosed by the invention, the technical advantages of having no wastes and saving energy are achieved.

Description

technical field [0001] The invention relates to a synthesis method of 5-chloro-2-phenoxyaniline and the used Beta molecular sieve. Background technique [0002] 5-Chloro-2-phenoxyaniline (CAS No.: 93-67-4) is an important intermediate of dyes and plays an important role in the research of organic synthesis and the industrial production of dyes. 5-Chloro-2-phenoxyaniline is usually condensed with 2,5-dichloronitrobenzene and phenol to synthesize 5-chloro-2-phenoxynitrobenzene and then reduced. [0003] The traditional preparation of 5-chloro-2-phenoxynitrobenzene is to dissolve 2,5-dichloronitrobenzene in a suitable solvent (such as o-dichlorobenzene), and then make phenol into potassium phenate or sodium phenate Aqueous solution, react at a certain temperature to produce 5-chloro-2-phenoxynitrobenzene. There are obvious defects in this process: firstly, the reaction temperature is relatively high, generally at 160-180°C, and a variety of non-target products are generated d...

Claims

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Application Information

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IPC IPC(8): C07C209/32C07C211/52B01J29/70
CPCB01J29/7007C07C201/12C07C209/32C07C205/38C07C211/52
Inventor 徐建成肖刚
Owner JINHUA SHUANGHONG CHEM CO LTD
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