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Synthesis technology of nitrophenol and intermediate thereof

A technology for nitrophenol and dinitrophenol, which is applied in the field of preparation of organic compounds, can solve the problems of substandard occupational hygiene, low safety, and large pollution, and achieves the effects of strong serial operability and avoiding large pollution.

Inactive Publication Date: 2017-06-20
JIUJIANG SHANSHUI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has the advantages of low pollution and high yield, but the disadvantage is that because the last step of the process is an acid-base neutralization process, a large amount of salt is inevitably trapped in the process of 2-amino-4-nitrophenol solid precipitation, resulting in 2- The active ingredient content of amino-4-nitrophenol is difficult to meet the production requirements of downstream products, so recrystallization and other treatments are required to treat 2-amino-4-nitrophenol
[0005] The invention discloses a synthesis process of nitrophenol and its intermediates. By simply modifying the substrate, the shortcomings of existing processes such as large pollution, low safety, substandard occupational health and low product quality are effectively avoided. , has the advantages of strong operability in series and high-quality products at one time

Method used

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  • Synthesis technology of nitrophenol and intermediate thereof
  • Synthesis technology of nitrophenol and intermediate thereof
  • Synthesis technology of nitrophenol and intermediate thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 184kg of 2,4-dinitrophenol was mixed with 79kg of acetyl chloride, 101kg of triethylamine, and 540kg of chloroform, and the reaction was completed to obtain 225kg of phenyl 2,4-dinitroacetate;

[0029] Mix 225kg 2,4-dinitroacetic acid phenyl ester with 450kg methanol, 0.67kg Pd / C, pass through hydrogen, 2,4-dinitroacetic acid phenyl ester is completely converted, and 181.5kg 2-amino-4 nitro Phenyl acetate;

[0030] By mixing 181.5 kg of 2-amino-4-nitrophenyl acetate with 185.2 kg of sodium hydroxide solution, the reaction was completed to obtain 140.6 kg of 2-amino-4-nitrophenol with a purity of 99.8%.

Embodiment 2

[0032] 184kg 2,4-dinitrophenol was mixed with 123kg isovaleryl chloride, 71.9kg potassium carbonate, and 368kg acetone, and the reaction was completed to obtain 266kg 2,4-dinitroisovalerate phenyl;

[0033] 266kg 2,4-dinitroisovalerate phenyl ester, 1064kg propyl acetate, 2.66kg Ru / C were mixed, the reaction was complete, and 207.9kg of 2-amino-4-nitroisovalerate phenyl ester with a purity of 98.7% was obtained .

Embodiment 3

[0035] By mixing 184kg 2,4-dinitrophenol with 123kg isovaleryl chloride, 71.9kg potassium carbonate, and 552kg dichloroethane, the reaction is completed to obtain 800kg 2,4-dinitroisovalerate phenyl dichloroethane solution ;

[0036] Through 800kg 2,4-dinitroisovalerate phenyl dichloroethane solution is mixed with 1.06kg Pd / C, stir until reaction is complete, obtain 2-amino-4-nitroisovalerate benzene of 221kg purity 99.7% ester.

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PUM

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Abstract

The invention relates to a synthesis technology of nitrophenol and an intermediate thereof, and discloses a synthesis method of 2-amino-4-nitrophenol. The synthesis method of 2-amino-4-nitrophenol comprises the following steps: 1, reacting 2-aminophenol (I) with hydrochloric acid or sulfuric acid in an organic solvent to synthesize a compound (II), and directly carrying out a next step reaction without recovering the organic solvent; 2, carrying out low temperature nitric acid nitration on the compound (II) in the organic solvent to obtain a compound (III), and ending the reaction; and 3, adding a liquid alkali to the above obtained system, distilling the system to recover the organic solvent, mixing the obtained distillation residue with an inorganic acid, carrying out solid-liquid separation to obtain a compound (IV), carrying out distilling concentration on the obtained mother liquor to obtain a commercial byproduct sodium chloride or sodium sulfate, and recovering distillation cooling water to use the distillation cooling water in the reaction. The chemical equation is shown in the description, and R in chemical equation is a chloride ion or a bisulfate ion. The technology has the advantages of high continuous operability, high safety, almost no wastes, realization of needed production devices being routine reaction devices, and easiness in realization of industrialization.

Description

technical field [0001] The invention relates to a preparation method of an organic compound, in particular to a synthesis process of nitrophenol and its intermediate. Background technique [0002] 2-Amino-4-nitrophenol, as a chemical synthesis intermediate, is widely used in dyes including reactive black ACE, neutral black BL / BRL / BGL and pharmaceutical products such as antihypertensive drugs acebutolol, 2-butyl -6-nitroindole and other production. [0003] The methods for synthesizing 2-amino-4-nitrophenol can be divided into electrochemical reduction and chemical reduction. Among them, chemical reduction includes general chemical reagent chemical reduction and metal catalytic hydrogenation reduction. Due to factors such as high production costs and lack of electrochemical facilities, the electrochemical reduction method has not yet reached the level of industrialization. At present, the chemical reduction method, especially the selective reduction of the 2-nitro group in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/00C07C215/76C07C219/34
CPCC07C213/00C07C201/12C07C215/76C07C219/34C07C205/42
Inventor 邵玉田冯宇周江平付居标王学泰何建武
Owner JIUJIANG SHANSHUI TECH
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