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Synthetic method of phenylhydrazine hydrochloride

A technology of phenylhydrazine hydrochloride and diazobenzene chloride, applied in the direction of hydrazine preparation and the like, can solve problems such as aggravating the economic burden of enterprises, affecting the growth of crops, damaging buildings and other facilities, etc. The effect of less waste water

Inactive Publication Date: 2016-02-24
WUHAN WUYAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

A large amount of reducing agent is used in the reaction, which produces a lot of salt wastewater, and the mixed salts are difficult to recycle, which seriously pollutes the water body. In addition, a large amount of sulfur dioxide gas is produced to pollute the atmosphere, forming acid rain and damaging the environment. plants, damage buildings and other facilities, and also cause soil compaction to affect the growth of crops. The treatment of waste water and waste gas will increase the economic burden of enterprises

Method used

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  • Synthetic method of phenylhydrazine hydrochloride
  • Synthetic method of phenylhydrazine hydrochloride
  • Synthetic method of phenylhydrazine hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0040] The preparation of embodiment 1 benzenediazonium chloride

[0041] Put 100 g of aniline (1.07 mol) and 326 g of 30% by mass hydrochloric acid (2.68 mol of HCl) into a 1 L flask, stir, and cool to 0° C. with an ice-water bath. The 406g mass percentage composition is 20% NaNO 2 Solution (1.18mol NaNO 2 ) is slowly poured into the solution in the above-mentioned flask, stirred, and incubated for 1.5 hours. Gained solution containing benzene diazonium chloride is designated as solution 1 # , analyzed with chromatographic detection, solution 1 # The benzenediazonium chloride yield obtained in is 142.7g.

[0042] Solution 2 # ~Solution 6 # The preparation operation is the same as solution 1 # , the difference lies in the ratio of raw materials and reaction conditions, solution 2 # With methanol as solvent, solution 3 # With ethanol as solvent. Solution 1 # ~Solution 6 # The ratio of raw materials and reaction conditions are shown in Table 2.

[0043] Table 2 prep...

Embodiment 2

[0045] Catalytic hydrogenation of benzenediazonium chloride in embodiment 2 tank reactor

[0046] Solution 1 # ~Solution 6 # The catalytic hydrogenation reaction of:

[0047] With the solution 1 that obtains in embodiment 1 # Added to the 5L tank type hydrogenation reactor. Add 9g of palladium-carbon catalyst into the kettle-type hydrogenation reactor, the hydrogenation pressure is 0.4MPa, and the reaction temperature is controlled at 30°C. After 2 hours of reaction, the material is discharged, and the filtrate is obtained by suction filtration under reduced pressure. Detected by chromatography, the total yield of phenylhydrazine hydrochloride reached 94%. Raw materials, reaction conditions and catalysts are as reaction number 1 in table 3 # shown.

[0048] Solution 2 # ~Solution 6 # Operation process of catalytic hydrogenation reaction with solution 1 # The difference is the type and amount of catalyst, and the reaction conditions are different. Its raw mat...

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Abstract

The invention discloses a method for synthesizing phenylhydrazine hydrochloride through catalytic hydrogenation. The method is characterized in that benzene diazonium chloride and a hydrogenation catalyst are contacted in the presence of hydrogen and the phenylhydrazine hydrochloride is prepared. With the adoption of the method, the solid catalytic hydrogenation catalyst is used, the reaction process is simplified, and the economy is substantially improved; meanwhile, the catalytic hydrogenation method is adopted, production of sulfur dioxide is avoided, the method is environment-friendly, less salt wastewater is produced and comprises the single component, and recovery and treatment are facilitated.

Description

technical field [0001] The application relates to a new synthesis process of a pyrazolone intermediate, which belongs to the technical field of pharmaceutical technology. Background technique [0002] Phenylhydrazine hydrochloride, Chinese name: phenylhydrazine hydrochloride, English name: Phenylhydrazinehydrochloride, is an important medicine, pesticide and dye intermediate, mainly used in the production of medicine pyrazolone, antipyrine, aminopyrine, Analgin is also used in dyes, pesticides and organic synthesis industries. It can also be used to detect chemical reagents such as vitamin B12, CO, Fe, Cu, Ni, etc. [0003] The existing production process is to use aniline as the main raw material, and carry out diazotization reaction with sodium nitrite at low temperature in acidic medium to generate diazotized benzene chloride, and then reduce it with ammonium sulfite and ammonium bisulfite to generate diazonium Sodium benzene disulfonate is analyzed by hydrochloric acid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C243/22C07C241/02
CPCC07C241/02C07C243/22
Inventor 皮金红赵涛涛董建强胡孟轲江雪娅张琦谢国范
Owner WUHAN WUYAO PHARMA
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