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Technological method for preparing m-aminophenol

A m-aminophenol and aminophenol technology, applied in the field of m-aminophenol preparation, can solve the problems of low yield and selectivity, high equipment requirements, serious pollution, etc., and achieve easy-to-obtain raw materials, high product yield, and simple operation Effect

Active Publication Date: 2018-01-09
山西智创药研科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, a variety of processes for the synthesis of m-aminophenol have been developed, mainly including nitrobenzene method, resorcinol ammonolysis method, m-nitrophenol electrolysis method, aniline hydroxylation method and m-phenylenediamine hydrochloric acid hydrolysis method, etc. , but most of them have the problems of backward technology, serious pollution, high cost, low yield and selectivity, and high requirements for equipment

Method used

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  • Technological method for preparing m-aminophenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A kind of processing method for preparing m-aminophenol in the present embodiment is carried out successively according to the following steps:

[0033] 1, the preparation of m-cresyl acetate of m-aminophenol reaction raw material:

[0034] A. The reaction equation is as follows:

[0035] C 7 h 8 O+CH 3 CClO→C 9 h 10 o 2 +HCl↑

[0036] B, the preparation steps are:

[0037] First, take m-cresol 21.6g in a 100ml Erlenmeyer flask, then add 15ml of dichloromethane as a solvent to the Erlenmeyer flask; secondly, under 1°C ice-water bath condition, use a constant pressure dropping funnel to dissolve 15.7g of acetyl chloride reagent Add it dropwise into the system, and fully react for 30 minutes; again, continue to react at a low temperature in an ice-water bath at 1°C for 60 minutes, then start to heat up, control the temperature of the system at 55°C, and react for 2 hours. The tail gas generated by the reaction is passed into an aqueous solution of sodium hydroxide...

Embodiment 2

[0056] A kind of processing method for preparing m-aminophenol, carries out successively according to the following steps:

[0057] 1, the preparation of m-cresyl acetate of m-aminophenol reaction raw material:

[0058] A. The reaction equation is as follows:

[0059] C 7 h 8 O+CH 3 CClO→C 9 h 10 o 2 +HCl↑

[0060] B, the preparation steps are:

[0061] First, take m-cresol 21.6g in a 100ml Erlenmeyer flask, then add 15ml of dichloromethane as a solvent to the Erlenmeyer flask; secondly, under 3°C ice-water bath conditions, use a constant pressure dropping funnel to dissolve 15.7g of acetyl chloride reagent Add it dropwise into the system, and fully react for 45 minutes; again, continue to react at a low temperature in an ice-water bath at 3°C ​​for 60 minutes, then start to heat up, control the temperature of the system at 60°C, and react for 2.5 hours. At last, the solid mixture generated after the reaction in the Erlenmeyer flask is taken out, and the unreacted sol...

Embodiment 3

[0080] A kind of processing method for preparing m-aminophenol, carries out successively according to the following steps:

[0081] 1, the preparation of m-cresyl acetate of m-aminophenol reaction raw material:

[0082] A. The reaction equation is as follows:

[0083] C 7 h 8 O+CH 3 CClO→C 9 h 10 o 2 +HCl↑

[0084] B, the preparation steps are:

[0085] First, take m-cresol 21.6g in a 100ml Erlenmeyer flask, and then add 15ml of dichloromethane as a solvent to the Erlenmeyer flask; secondly, under 5°C ice-water bath conditions, use a constant pressure dropping funnel to dissolve 15.7g of acetyl chloride reagent Add it dropwise into the system, and fully react for 60 minutes; again, continue to react at a low temperature of 5°C in an ice-water bath for 60 minutes, then start to heat up, control the temperature of the system at 65°C, and react for 3 hours. The tail gas generated by the reaction is passed into the sodium hydroxide aqueous solution At last, the solid mixt...

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Abstract

The invention relates to a technological method for preparing m-aminophenol, belongs to the technical field of chemical material preparation and solves the technical problem of limit caused by utilizing phenyl acetate as a preparation raw material. The technological method disclosed by the invention has the advantages of simpleness in operation, high product yield, reaction easy to control and thelike. The technological method is characterized by comprising the steps: preparing 3-carboxyphenyl phenyl acetate after preparing m-cresyl acetate and utilizing the prepared 3-carboxyphenyl phenyl acetate to prepare the m-aminophenol. The technological method comprises the steps: a, taking a C9H8O4 solvent, adding into an ethyl acetate solution, fully stirring until complete dissolution, dropwiseadding thionyl chloride into a system under the ice water bath condition, thermally insulating 1+ / -0.5 hours, warming to 60 DEG C and refluxing; b, under the ice water bath condition, adding triethylamine and hydroxylamine hydrochloride into the system, thermally insulating for 2 hours and warming to a room temperature; c, spin drying the solvent on a rotary evaporator, then adding water and potassium carbonate, warming to 60 to 70 DEG C and hydrolyzing; d, utilizing ethyl acetate to extract the solution, utilizing a thin-layer chromatography to determine whether extraction is complete and obtaining the finished product of the m-aminophenol after the extraction is finished.

Description

technical field [0001] The invention belongs to the technical field of chemical material preparation, in particular to a process for preparing m-aminophenol. Background technique [0002] Meta-aminophenol is an important fine chemical raw material and organic intermediate, which is widely used in petrochemical industry, pesticide, medicine, dyestuff and other fields. So far, a variety of processes for the synthesis of m-aminophenol have been developed, mainly including nitrobenzene method, resorcinol ammonolysis method, m-nitrophenol electrolysis method, aniline hydroxylation method and m-phenylenediamine hydrochloric acid hydrolysis method, etc. , but most of them have the problems of backward technology, serious pollution, high cost, low yield and selectivity, and high requirements for equipment. Contents of the invention [0003] The object of the present invention is to overcome the defective of prior art, a kind of processing method of preparing m-aminophenol is prov...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/00C07C213/02C07C215/76
Inventor 游成海李兴李鸿胡志敏牛茹茹崔喜牛鑫曲军
Owner 山西智创药研科技有限公司
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