Preparation technology of high purity 3-hydroxyacetophenone

A technology for hydroxyacetophenone and preparation process, which is applied in the preparation of carbon-based compounds, preparation of organic compounds, organic chemistry and other directions, can solve the problems of low product purity, low product yield and high production cost, and achieves high product purity, The effect of high product yield and reduced production cost

Active Publication Date: 2011-11-23
XIANTAO XIANSHENG FINE CHEM
View PDF2 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention mainly solves the technical problems such as low product purity, low product yield, hig

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation technology of high purity 3-hydroxyacetophenone
  • Preparation technology of high purity 3-hydroxyacetophenone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: Add 36 parts by weight of 3-nitroacetophenone, 0.03 parts by weight of methanol and 36 parts by weight of water into the reaction kettle, and then slowly add 22 parts by weight of iron powder to react for 10 hours after heating to 95°C After the filtrate enters the receiving tank, it is gradually cooled to 30°C after 10 hours. The precipitate is centrifuged to remove water and 3-aminoacetophenone is obtained (the centrifugal water is fully recovered and recycled as the reaction water for the next feeding ); Pour the obtained 3-aminoacetophenone into the diazonium kettle, add 8 parts by weight of 98% sulfuric acid, cool to 10°C, and then slowly add 8 parts by weight of sodium nitrite aqueous solution to the diazonium kettle After adding in 15 hours, 3-diazosulfate acetophenone is obtained; add 19 parts by weight of water to the hydrolysis kettle, and then increase the temperature to 95° C. to obtain 3-diazosulfate acetophenone Slowly added to the hydrolysis ket...

Embodiment 2

[0015] Example 2: Add 38 parts by weight of 3-nitroacetophenone, 0.03 parts by weight of methanol and 37 parts by weight of water into the reaction kettle, and slowly add 21 parts by weight of iron powder to react for 10 hours after heating to 95°C After the filtrate enters the receiving tank, it is gradually cooled to 30°C after 10 hours. The precipitate is centrifuged to remove water and 3-aminoacetophenone is obtained (the centrifugal water is fully recovered and recycled as the reaction water for the next feeding ); Pour the obtained 3-aminoacetophenone into the diazonium kettle, add 6 parts by weight of 98% sulfuric acid, cool to 5°C, and then slowly add 7 parts by weight of sodium nitrite aqueous solution to the diazonium kettle After adding in 15 hours, 3-diazosulfate acetophenone was prepared; 18 parts by weight of water was added to the hydrolysis kettle, and then the temperature was raised to 95°C, and the obtained 3-diazosulfate acetophenone The ketone was slowly add...

Embodiment 3

[0016] Example 3: Add 37 parts by weight of 3-nitroacetophenone, 0.04 parts by weight of methanol and 38 parts by weight of water into the reaction kettle, and slowly add 20 parts by weight of iron powder to react for 10 hours after heating to 95°C After the filtrate enters the receiving tank, it is gradually cooled to 30°C after 10 hours. The precipitate is centrifuged to remove water and 3-aminoacetophenone is obtained (the centrifugal water is fully recovered and recycled as the reaction water for the next feeding ); Pour the obtained 3-aminoacetophenone into the diazonium kettle, add 7 parts by weight of 98% sulfuric acid, cool to 8°C, and then slowly add 6 parts by weight of sodium nitrite aqueous solution to the diazonium kettle After adding in 15 hours, 3-diazosulfate acetophenone is obtained; add 17 parts by weight of water to the hydrolysis kettle, and then increase the temperature to 95° C. to obtain 3-diazosulfate acetophenone Slowly add to the hydrolysis kettle, aft...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
Melting pointaaaaaaaaaa
Login to view more

Abstract

A preparation technology of high purity 3-hydroxyacetophenone comprises the following steps of: adding 38 weight portions of 3-nitroacetophenone and 37 weight portions of water into a reaction vessel, adding an iron powder to react for 10 hours, adding methanol with stirring, centrifuging a precipitate for removing water to obtain 3-aminoacephenone, pouring the 3-aminoacephenone into a diazonium kettle; adding sulfuric acid, slowly adding a sodium nitrite aqueous solution into the diazonium kettle to produce 3-diazo sulfate acetophenone, adding 3-diazo sulfate acetophenone into a hydrolysis kettle, and finally drying to obtain the pure product 3-hydroxyacetophenone. The invention has advantages of simple technology, high yield of the product and high purity. By reasonable design of the reaction steps and adjustment of charging order, the application amount of strong acid is greatly reduced; in addition, by the addition of a certain amount of methanol in the reaction, the process of the reaction can be accelerated and the synthesis quality can be raised. According to statistics, the overall yield of the technology can reach over 92%; compared with other production technologies, the technology provided by the invention enables the product cost to decrease by more than 40%, and is environmentally friendly.

Description

Technical field [0001] The invention relates to a production technology of 3-hydroxyacetophenone, in particular to a preparation technology of high-purity 3-hydroxyacetophenone. Background technique [0002] 3-Hydroxyacetophenone (m-hydroxyacetophenone) is an important intermediate for the preparation of new medicine phenylephrine. The existing production process is as follows: [0003] a. Add 3-nitroacetophenone and water into the reaction tank, add iron powder while stirring, slowly add hydrochloric acid, heat to 90℃ and reflux for 6-8 hours, cool to 30℃, and add hydrochloric acid to make the reaction liquid strong Acidic, then filter, take the filtrate and add ammonia water until it is weakly alkaline, and then precipitate solids, and filter the solids to obtain 3-aminoacetophenone; [0004] b. Add water and concentrated hydrochloric acid into the reaction pot, add 3-aminoacetophenone with stirring, then lower the temperature to 5-10°C, add dropwise sodium nitrite aqueous soluti...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07C49/825C07C45/64
Inventor 邵新华
Owner XIANTAO XIANSHENG FINE CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap