Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Process of preparing beta-p-hydroxyphenyl ethanol

A technology of p-hydroxyphenylethanol and p-alkoxybenzene, which is applied in the direction of hydrolysis preparation, etc., can solve the problems of complex process, high risk of use, and difficult separation of by-products, and achieve the effect of simple operation and low cost

Inactive Publication Date: 2007-11-07
ZHEJIANG APELOA MEDICAL TECH
View PDF5 Cites 8 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the haloalkylation step of this method, due to the selectivity of the haloalkane on the benzene ring, the final by-product is difficult to separate, which brings certain difficulties to the purification of the product.
[0007] In summary, there are many methods for synthesizing β-hydroxyphenylethanol, but there are generally defects such as high raw material prices, high requirements for reaction conditions, high risk of use, complicated process, and difficulty in industrialized production.

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
  • Process of preparing beta-p-hydroxyphenyl ethanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Stir the crude p-methoxyphenylethanol to raise the temperature under reduced pressure, rectify under reduced pressure through a rectification column, and collect fractions at 150°C-230°C at a vacuum degree of -0.085MPa. The content of p-methoxyphenethyl alcohol after rectification is more than 98% through gas chromatography analysis, and its single impurity is not higher than 1.0%.

[0024] According to the molar ratio of p-methoxyphenethyl alcohol: hydrochloric acid: water: dichloromethane = 1: 0.30: 1.7: 1.5, the rectified p-methoxyphenethyl alcohol, hydrochloric acid and dichloromethane are mixed, wherein the hydrochloric acid is pre-configured into a 3% aqueous solution, and then add the remainder of water.

[0025] Carry out the hydrolysis reaction at 30°C for 4 hours, and control the vacuum degree at -0.03~-0.05MPa. After the hydrolysis reaction is completed and the vacuum is broken, the temperature is lowered to 0°C, and an appropriate amount of seed crystals are...

Embodiment 2

[0027] Stir the crude p-ethoxyphenethyl alcohol, raise the temperature under reduced pressure, and rectify under reduced pressure through a rectification column, and collect fractions at 150°C-230°C when the vacuum degree is greater than -0.085MPa. The content of p-ethoxyphenethyl alcohol after rectification is more than 98% through gas chromatography analysis, and its single impurity is not higher than 1.0%.

[0028] P-ethoxyphenethyl alcohol: sulfuric acid: water: dichloroethane=1: 0.35: 1.8: 1.8 according to the molar ratio, the rectified p-ethoxyphenethyl alcohol, sulfuric acid and dichloroethane are mixed, wherein the sulfuric acid Pre-configured as a 4% aqueous solution, and then add the balance of water.

[0029] Carry out the hydrolysis reaction at 60°C for 2 hours, and control the vacuum at -0.04~-0.06MPa. After the hydrolysis reaction is completed and the vacuum is broken, the temperature is lowered to 5°C, and an appropriate amount of seed crystals are added to the ...

Embodiment 3

[0031] Stir the crude p-isopropoxyphenylethanol to increase the temperature under reduced pressure, and rectify it through a rectification column under reduced pressure, and collect fractions at 150°C-230°C when the vacuum degree is greater than -0.085MPa. The content of p-isopropoxyphenethyl alcohol after rectification is more than 98% through gas chromatography analysis, and its single impurity is not higher than 1.0%.

[0032] According to the molar ratio of p-isopropoxyphenethyl alcohol: hydrochloric acid: water: chloroform = 1: 0.4: 2.0: 1.7, the rectified p-isopropoxyphenethyl alcohol, hydrochloric acid and chloroform are mixed, wherein the hydrochloric acid is pre-configured to 10 % aqueous solution, and then add the remainder of water.

[0033] Carry out the hydrolysis reaction at 50°C for 5 hours, and control the vacuum degree at -0.04~-0.06MPa. After the hydrolysis reaction is completed and the vacuum is broken, the temperature is lowered to 2°C, and an appropriate a...

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

No PUM Login to View More

Abstract

The present invention discloses process of synthesizing beta-p-hydroxyphenyl ethanol. The materials including p-alkoxyphenyl ethanol, inorganic acid, water and organic solvent in the molar ratio of 1 to 0.28-0.5 to 1.7-2.0 to 1-2 are first made to produce hydrolysis reaction at 30-60 deg.c for 2-4 hr; the hydrolysis product is cooled to 0-8 deg.c to separate out crystal; and the crystal is post-treated to obtain beta-p-hydroxyphenyl ethanol. The beta-p-hydroxyphenyl ethanol preparing process of the present invention has simple operation and low cost, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the synthesis technology of fine chemicals, in particular to a preparation method of β-p-hydroxyphenethyl alcohol, and belongs to the field of medicine and chemical industry. Background technique [0002] β-p-Hydroxyphenethyl alcohol is an important pharmaceutical intermediate, and the synthetic methods in the prior art include: [0003] European patent EP0449603 and US patent US5003115 introduce the use of 4-acetoxystyrene as a raw material, the oxidation of peroxycarboxylic acid, hydrogen reduction reaction, and saponification reaction to prepare β-p-hydroxyphenylethanol. This method is owing to adopting 4-acetoxy styrene as raw material, makes this synthetic reaction have better initial condition, but 4-acetoxy styrene is not commonly used common organic compound, if prepare β-para Hydroxyphenethyl alcohol can be difficult to obtain because of raw material, makes this synthetic method be difficult to realize the needs of in...

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): C07C39/11C07C29/10
Inventor 雷江郑毓李海青李星梅文军徐宏烈
Owner ZHEJIANG APELOA MEDICAL TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com