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Method for synthesizing 2-(4-benzylmethoxyphenyl)ethanol medical intermediate

A technology of benzyloxyphenyl and synthetic method, which is applied in the field of synthesis of pharmaceutical intermediate 2-ethanol, can solve the problems of many by-products, low product yield, long reaction route, etc., and achieve few by-products and high yield High, easy-to-operate effect

Inactive Publication Date: 2014-09-03
江苏德峰药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional 2-(4-benzyloxyphenyl)ethanol manufacturing process has a long reaction route, cumbersome process, and many by-products, resulting in low product yield and poor production efficiency.

Method used

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  • Method for synthesizing 2-(4-benzylmethoxyphenyl)ethanol medical intermediate
  • Method for synthesizing 2-(4-benzylmethoxyphenyl)ethanol medical intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] (1) Synthesis of crude product

[0013] Add 200ml of water and 50g of 4-hydroxyphenylethanol into a 1000ml three-necked bottle, stir and mix well at room temperature, add dropwise the pre-configured potassium hydroxide solution (20g potassium hydroxide + 100ml water), and the dropping time is 0.5h- After 1h, the dripping was completed, and the water was distilled off under reduced pressure. When the evaporation of water was about 250ml, the evaporation was stopped; the above solution was transferred to a rotary evaporator, and spin-dried until the water content was less than 0.1%. Then, 300ml of toluene and 50g of silica gel were added. When the temperature does not exceed 30°C, add 50g of benzyl chloride dropwise, raise the temperature to 108°C under reflux, and keep it under reflux for 30 hours. After the reaction is over, add 200ml of toluene, heat filter, add 200ml of water, heat up and stir, and heat up to 50°C. Stir left and right for half an hour and let it stand...

Embodiment 2

[0017] (1) Synthesis of crude product

[0018] The crude process is the same as in Example 1, except that 100 grams of molecular sieves are used instead of the above 50 grams of silica gel, and the obtained crude product has a wet weight of 88.5 g and a dry weight of 74.9 g.

[0019] (2) refined

[0020] 74.9g of crude product was refined, its crystal wet weight was 69.9g, dry weight was 64.9g, the product was white crystal, its yield was 78.5%, and its content was 99.6%.

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Abstract

The invention discloses a 2-(4-benzylmethoxyphenyl)ethanol medical intermediate, which comprises the following steps of: mixing and stirring p-hydroxyphenethyl ethanol and water uniformly; dripping an aqueous solution of potassium hydroxide to form potassium 4-hydroxyphenethyl ethoxide; removing water in the salt, adding toluene and water absorbent at a temperature of not higher than 30DEG C; dripping benzyl chloride to form coarse 2-(4-benzylmethoxyphenyl)ethanol; and refining the coarse product to obtain the target product. The method has the advantages of simplicity in operation, fewer byproducts, and high yield. The 2-(4-benzylmethoxyphenyl)ethanol content of the finished products is 99.6%, and the yield of the 2-(4-benzylmethoxyphenyl)ethanol medical intermediate is 60-85%.

Description

technical field [0001] The invention relates to a method for synthesizing a pharmaceutical intermediate 2-(4-benzyloxyphenyl)ethanol. Background technique [0002] 2-(4-Benzyloxyphenyl)ethanol, the molecular formula is C 15 h 16 o 2 , is an important organic chemical product, mainly used in the fields of high-end fine chemicals such as medicine, pesticides, and new materials. The traditional 2-(4-benzyloxyphenyl)ethanol manufacturing process has a long reaction route, cumbersome process, and many by-products, resulting in low product yield and poor production efficiency. Contents of the invention [0003] The purpose of this invention is to provide a kind of synthetic method of 2-(4-benzyloxyphenyl) ethanol with high yield, low cost and easy operation. [0004] In order to solve the above-mentioned technical problems, the technical scheme adopted in the present invention is: a kind of synthetic method of pharmaceutical intermediate 2-(4-benzyloxyphenyl)ethanol, it is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/23C07C41/16
Inventor 王德峰俞健钧王炳才
Owner 江苏德峰药业有限公司