Preparation method of magnesium mono-p-nitrobenzyl malonate

A technology of nitrobenzyl malonate and p-nitrobenzyl alcohol, which is applied in the field of medicine, can solve the problems of low product yield, many by-products, and high production costs, and achieve high purity, few by-products, and high production low cost effect

Inactive Publication Date: 2014-01-01
NORTH CHINA UNIV OF WATER RESOURCES & ELECTRIC POWER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of this invention is to provide a kind of preparation method of p-nitrobenzyl alcohol malonate monoester magnesium, which solves the problems of many by-products, low product yield and high production cost in the preparation process of magnesium reagent

Method used

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Experimental program
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Effect test

Embodiment 1

[0023] The preparation method of the p-nitrobenzyl alcohol malonate monoester magnesium of the present embodiment may further comprise the steps:

[0024] 1) According to the molar ratio of p-nitrobenzyl alcohol and malonic acid as 1:1, add p-nitrobenzyl alcohol and malonic acid to benzene, and perform esterification at -18°C in the presence of a catalyst Reaction, the time of esterification reaction is 60min; The mol ratio of described catalyzer is sulfuric acid and phosphoric acid is the mixed acid of 1:1, and the add-on of described catalyzer is 0.5% of p-nitrobenzyl alcohol adding quality;

[0025] 2) After the esterification reaction is completed, the temperature of the reaction system is raised to 70°C, so that the crystal form of the reaction product undergoes transformation, and p-nitrobenzyl malonate monoester is obtained;

[0026] 3) Add p-nitrobenzyl alcohol malonate monoester and magnesium chloride obtained in step 2) into water at a molar ratio of 0.6:1 for reacti...

Embodiment 2

[0028] The preparation method of the p-nitrobenzyl alcohol malonate monoester magnesium of the present embodiment may further comprise the steps:

[0029] 1) According to the molar ratio of p-nitrobenzyl alcohol and malonic acid as 1:1.5, add p-nitrobenzyl alcohol and malonic acid into acetone, and perform esterification at -10°C in the presence of a catalyst Reaction, the time of esterification reaction is 50min; The mol ratio of described catalyzer is sulfuric acid and phosphoric acid is the mixed acid of 1:1, and the add-on of described catalyzer is 1.5% of p-nitrobenzyl alcohol adding quality;

[0030] 2) After the esterification reaction is completed, the temperature of the reaction system is raised to 60°C, so that the reaction product undergoes crystal transformation to obtain p-nitrobenzyl malonate monoester;

[0031] 3) Add p-nitrobenzyl alcohol malonate monoester and magnesium chloride obtained in step 2) into water at a molar ratio of 0.5:1 for reaction, and the rea...

Embodiment 3

[0033] The preparation method of the p-nitrobenzyl alcohol malonate monoester magnesium of the present embodiment may further comprise the steps:

[0034] 1) According to the molar ratio of p-nitrobenzyl alcohol and malonic acid as 1:2, add p-nitrobenzyl alcohol and malonic acid into acetone, and perform esterification at -15°C in the presence of a catalyst Reaction, the time of esterification reaction is 40min; The mol ratio of described catalyzer is sulfuric acid and phosphoric acid is the mixed acid of 1:1, and the add-on of described catalyzer is 2% of p-nitrobenzyl alcohol adding quality;

[0035] 2) After the esterification reaction is completed, the temperature of the reaction system is raised to 75°C, so that the crystal form of the reaction product undergoes transformation, and p-nitrobenzyl malonate monoester is obtained;

[0036] 3) Add p-nitrobenzyl alcohol malonate monoester and magnesium chloride obtained in step 2) into water at a molar ratio of 0.8:1 for reacti...

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Abstract

The invention discloses a preparation method of magnesium mono-p-nitrobenzyl malonate. The preparation method comprises following steps: 1) 1-hydroxymethyl-4-nitrobenaene and malonic acid are added into a solvent, and the solution is subjected to esterification at a low temperature and in the presence of a catalyst; 2) the temperature of the reaction system is increased to 60 to 80 DEG C so as to realized crystal transition of products, and obtain mono-p-nitrobenzyl malonate; and 3) mono-p-nitrobenzyl malonate obtained in step 1) and magnesium chloride are added into water for reaction, and the reaction product is subjected to recrystallization, centrifugal separation and drying process so as to obtain magnesium mono-p-nitrobenzyl malonate. According to the preparation method, purity of intermediate mono-p-nitrobenzyl malonate is high, and can be more than 95%; yield of magnesium mono-p-nitrobenzyl malonate is high, and can be more than 80%; product clarity after dissolving is high; raw materials are easily available; reaction conditions are mild; operation is simple and convenient; by-products are few; production cost is low; and the preparation method is suitable for large-scaled industrialized production.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of magnesium p-nitrobenzyl malonate monoester. Background technique [0002] With the widespread use of penicillin and cephalosporin β-lactam antibiotics, antibodies to these antibiotics are gradually produced in the human body; the drug resistance of bacterial strains is also gradually enhanced, resulting in an increasing amount of clinical medication and various side effects. In recent years, most of the new β-lactam antibiotics studied are modified side chains. Although these antibiotics have bactericidal effect on Gram-positive bacteria (including Gram-negative bacteria of Pseudomonas aeruginosa), in order to avoid It is decomposed by enzymes in the kidneys in the body, and when this type of antibiotic is used in combination with an inhibitor of this enzyme, it will produce toxicity that affects the kidneys and central nervous system. [000...

Claims

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Application Information

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IPC IPC(8): C07C205/42C07C201/12
Inventor 刘秉涛郭毅萍李新奇姚文志
Owner NORTH CHINA UNIV OF WATER RESOURCES & ELECTRIC POWER
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