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Preparation method of 4-methoxybenzyl chloride

A technology of methoxybenzyl chloride and benzyl alcohol, applied in the field of antibiotic drug synthesis, can solve the problems of dark color of 4-methoxybenzyl chloride, high toxicity of solvent acetone, complicated post-processing, etc., achieve complete reaction and reduce energy consumption , the effect of easy operation

Inactive Publication Date: 2017-09-15
山西千岫制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The 4-methoxybenzyl chloride obtained in the above-mentioned reaction process has a darker color, lower purity, and complicated aftertreatment. In addition, the solvent acetone used is more toxic and pollutes the environment.

Method used

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  • Preparation method of 4-methoxybenzyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Put 30g of white hydrochloric acid into a clean and rust-free reaction kettle, cool down to 0~-5°C, add 9.6g of p-methoxybenzyl alcohol, and stir for 10min at a temperature of 11°C, send the sample and stir slowly, and pass the test immediately Let it stand still for 30 minutes, separate the liquid, discard the upper layer, add Yuanming powder to the lower layer, stir for 30 minutes, filter to obtain 4-methoxybenzyl chloride, and store it in isolation from the air for later use.

Embodiment 2

[0027] Put 30g of white hydrochloric acid into a clean and rust-free reaction kettle, cool down to 0~-5°C, add 11g of p-methoxybenzyl alcohol, stir for 10min at a temperature of 11°C, and slow down the stirring when sending samples. Let it stand for 30 minutes, separate the liquid, discard the upper layer, add Yuanming powder to the lower layer, stir for 30 minutes, filter to obtain 4-methoxybenzyl chloride, and keep it isolated from the air for later use.

Embodiment 3

[0029] Put 30g of white hydrochloric acid into a clean and rust-free reaction kettle, cool down to 0~-5°C, add 12.0g of p-methoxybenzyl alcohol, and stir for 13min at a temperature of 12°C, send the sample slowly and stir, and pass the test Immediately let it stand still for 40 minutes, separate the liquid, discard the upper layer, add Yuanming powder to the lower layer, stir for 35 minutes, filter to obtain 4-methoxybenzyl chloride, and keep it isolated from the air for later use.

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Abstract

The invention discloses a preparation method of 4-methoxybenzyl chloride. The method comprises the following steps: adding hydrochloric acid, and cooling the hydrochloric acid; adding 4-methoxybenzyl alcohol; carrying out a reaction, and carrying out liquid separation; drying the obtained liquid; and filtering the dried liquid to obtain the target compound. The method has the advantages of extremely easily controlled reaction temperature, completeness in reaction, few impurities, realization of high purity reaching 99%, high yield reaching 90-95%, colorlessness and transparence of the obtained product, simplicity in operation, reduction of the device investment, and reduction of the energy consumption.

Description

technical field [0001] The invention belongs to the technical field of antibiotic drug synthesis, and in particular relates to a preparation method of 4-methoxybenzyl chloride. Background technique [0002] 4-Methoxybenzyl chloride, alias: p-methoxybenzyl chloride, p-methoxybenzyl chloride, 4-methoxybenzyl chloride; molecular formula C8H9ClO, CAS number: 824-94-2, molecular weight: 156.6095, melting point − 1°C, boiling point 117-118 °C14 mm Hg, density 1.155 g / ml at 25 °C. Its molecular structural formula is: [0003] The synthesis of 4-methoxybenzyl chloride is the first step in the preparation method of the 7-position side chain acid of latamoxef, and the 7-position side chain acid of latamoxef is a key intermediate prepared by latamoxef drugs, It can also be used for other purposes by taking advantage of its benzyl chloride properties. The current synthesis steps of 4-methoxybenzyl chloride are as follows: at room temperature, slowly add concentrated hydrochloric ac...

Claims

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Application Information

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IPC IPC(8): C07C41/22C07C43/225
CPCC07C41/22C07C43/225
Inventor 王作弟
Owner 山西千岫制药有限公司