A kind of synthetic method of p-hydroxyphenethyl alcohol

A technology for p-hydroxyphenethyl alcohol and a synthesis method, which is applied in the field of synthesis of p-hydroxyphenethyl alcohol, can solve the problems of high raw material cost, strict requirements on production equipment and raw materials, complicated processes, etc., and achieves simple and mild reaction conditions, low cost, and high efficiency. Handling simple effects

Active Publication Date: 2022-07-15
杭州盛弗泰新材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the yield of this synthesis process is high, its disadvantages are that the cost of raw materials is too high, the process is complicated, and the requirements for production equipment and raw materials are strict.
Therefore, the application in actual mass production is greatly limited.

Method used

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  • A kind of synthetic method of p-hydroxyphenethyl alcohol

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preparation example Construction

[0032] A kind of synthetic method of p-hydroxyphenethyl alcohol, comprises the following steps:

[0033] 1) Add methanol, sodium methoxide and a catalyst into the reactor and stir; the catalyst is selected from potassium iodide and cuprous iodide; the amount of the catalyst is 0.05-0.1 times the mass of 4-chlorophenethyl alcohol.

[0034] 2) 4-chlorophenethyl alcohol is added into the above-mentioned reactor in batches, and the temperature is raised to the reflux temperature for reaction; the consumption of methanol is 3-6 times of the quality of 4-chlorophenethyl alcohol. The molar ratio of sodium methoxide and 4-chlorophenethyl alcohol is 5-10:1.

[0035] 3) The solution obtained after the reaction in step 2) is lowered to room temperature, filtered, and the filtrate is evaporated to dryness to obtain a crude 4-methoxyphenethyl alcohol;

[0036] 4) adding the crude 4-methoxyphenethyl alcohol obtained in step 3) into another reactor, adding a solvent, and stirring; the solve...

Embodiment 1

[0041] 1) Add 15kg of methanol, 5.4kg of sodium methoxide and 0.23kg of CuI to the reactor at room temperature to start stirring.

[0042] 2) 3.13 kg of 4-chlorophenethyl alcohol was added to the above mixed solution in batches, and heated to about 80 degrees to reflux.

[0043] 3) The material was cooled to room temperature, filtered, and the filtrate was spin-dried to obtain crude 4-methoxyphenethyl alcohol: 3kg.

[0044] 4) Add the obtained material into the reaction kettle, add 15kg of glacial acetic acid, and stir at room temperature.

[0045] 5) wherein drip 47% hydrobromic acid 10.3kg, be warming up to 116 ℃, be incubated and refluxed.

[0046] 6) Sampling detection, 4-methoxyphenethyl alcohol reaction is completed, and it is cooled to about 60 DEG C. Slowly add 20% sodium carbonate solution dropwise to the material while observing the pH value of the reaction. When the pH value is between 6-7, stop dripping.

[0047] 7) Continue the insulation reaction for 2h, be c...

Embodiment 2

[0050] 1) Add 15kg of methanol, 8.6kg of sodium methoxide and 0.27kg of KI to the reactor at normal temperature to start stirring.

[0051] 2) 3.13 kg of 4-chlorophenethyl alcohol was added to the above mixed solution in batches, heated to about 84 degrees and refluxed.

[0052] 3) The material was cooled to room temperature, filtered, and the filtrate was spin-dried to obtain crude 4-methoxyphenethyl alcohol: 2.96 kg.

[0053] 4) Add the obtained material into the reaction kettle, add 17.7kg of glacial acetic acid, and stir at room temperature.

[0054] 5) wherein drip 12.1kg of 40% hydrobromic acid, be warming up to 116 ℃, be incubated and refluxed.

[0055] 6) Sampling detection, 4-methoxyphenethyl alcohol reaction is completed, and it is cooled to about 60 DEG C. Slowly add 10% sodium hydroxide solution dropwise to the material while observing the pH value of the reaction. When the pH value is between 6-7, stop dripping.

[0056]7) Continue the insulation reaction for ...

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Abstract

The invention relates to the field of organic synthesis, and discloses a method for synthesizing p-hydroxyphenethyl alcohol. Evaporate to dryness to obtain the 4-methoxyphenethyl alcohol crude product; 4) add the crude product to the solvent and stir; 5) dropwise add hydrobromic acid, heat up and reflux, and keep the temperature for the reaction until the reaction is complete; 6) be cooled to 55-65 ° C , slowly add alkaline solution, adjust the pH value to 6-7; 7) cool down to 8-12 ° C, stir for 0.5-1.5h, filter the material to obtain a wet filter cake, add a solvent, heat up to dissolve, separate water, and recrystallize , filtered, and spin-dried to obtain the final product. The purity of the product of the method of the invention can reach more than 99%, the yield can reach more than 90%, and the reaction conditions of the whole synthesis process are simple and mild, the post-processing is simple, and the cost is low.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing p-hydroxyphenethyl alcohol. Background technique [0002] p-Hydroxyphenethyl alcohol is an important fine chemical intermediate, which has a wide range of uses in the pharmaceutical and perfume industries, mainly for the synthesis of metoprolol, betaxolol, salidroside, maltine, etc. [0003] The chemical synthesis methods of p-Hydroxyphenethyl mainly include the following: 1. Phenethylamine synthesis method; 2. Phenethyl alcohol synthesis method; 3. Phenol synthesis method; 4. P-Bromophenol synthesis method; 5. P-Hydroxyphenethyl ester Reduction method; 6, p-nitrophenylacetic acid method, etc. [0004] The above several synthetic methods have their own advantages and disadvantages: some raw materials are simple in source, but the process conditions are complicated; some raw materials are expensive and difficult to industrialize; some have many three was...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/055C07C37/02C07C39/11
CPCC07C41/16C07C37/055C07C37/02C07C43/23C07C39/11
Inventor 刘文龙
Owner 杭州盛弗泰新材料科技有限公司
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