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
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  • 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 ar

Method used

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  • Process of preparing beta-p-hydroxyphenyl ethanol

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Experimental program
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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...

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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

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Application Information

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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
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