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3-Hydroxyl-4-nitrobenzoic acid and preparation method thereof

A technology of nitrobenzoic acid and hydroxyl, which is applied in the field of biomedicine, can solve problems such as the need to improve the yield, and achieve the effect of easy operation, easy implementation, and simple steps

Inactive Publication Date: 2016-06-15
叶芳
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But specifically to the p-nitrobenzoic acid derivatives substituted by the 3-hydroxyl group, due to the particularity of the hydroxyl group, the yield in the preparation process still needs to be improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 108g (1mol) of m-cresol, 0.2mol of metal lithium and 1L of concentrated sulfuric acid into the reaction kettle, stir at 40°C, add 400mL of concentrated nitric acid dropwise, after the dropwise addition is completed, continue the reaction for 2 hours, and then steam out 5 -Methyl-2-nitrophenol, dissolve the produced 5-methyl-2-nitrophenol in 1.7L absolute ethanol and add it to the reaction kettle, maintain the temperature at 55°C, add 2.5molH 2 o 2 , stirring at a speed of 40-60 rev / min, controlling the pressure at 1.2Mpa, after continuing the reaction for 2h, removing absolute ethanol and H 2 o 2 , After steaming to remove impurities, yellow crystals were precipitated, and after drying, the target product 3-hydroxy-4-nitrobenzoic acid was obtained.

[0019] The purity of the obtained 3-hydroxy-4-nitrobenzoic acid was 92.4%, and the yield was 90.2%.

Embodiment 2

[0021] Add 108g (1mol) of m-cresol, 0.25mol of metal lithium and 700mL of concentrated sulfuric acid into the reaction kettle, stir at 45°C, add 350mL of concentrated nitric acid dropwise, after the dropwise addition, continue the reaction for 2h, and then steam out 5 -Methyl-2-nitrophenol, dissolve the produced 5-methyl-2-nitrophenol in 1.9L absolute ethanol and add it to the reaction kettle, maintain the temperature at 55°C, add 2.3molH 2 o 2 , stirred at a speed of 50 rev / min, controlled the pressure at 1.5Mpa, and continued to react for 2 hours to remove absolute ethanol and H 2 o 2 , After steaming to remove impurities, yellow crystals were precipitated, and after drying, the target product 3-hydroxy-4-nitrobenzoic acid was obtained.

[0022] The purity of the obtained 3-hydroxy-4-nitrobenzoic acid was 90.7%, and the yield was 91.8%.

Embodiment 3

[0024] Add 108g (1mol) of m-cresol, 0.3mol of metal lithium and 900mL of concentrated sulfuric acid into the reaction kettle, stir at 50°C, add 500mL of concentrated nitric acid dropwise, after the dropwise addition, continue the reaction for 2h, and then steam out 5 -Methyl-2-nitrophenol, dissolve the produced 5-methyl-2-nitrophenol in 2.1L absolute ethanol and add it to the reaction kettle, maintain the temperature at 55°C, add 2.0molH 2 o 2 , stirred at a speed of 45 rev / min, controlled the pressure at 1.3Mpa, and continued to react for 2 hours to remove absolute ethanol and H 2 o 2 , After steaming to remove impurities, yellow crystals were precipitated, and after drying, the target product 3-hydroxy-4-nitrobenzoic acid was obtained.

[0025] The purity of the obtained 3-hydroxy-4-nitrobenzoic acid was 94.7%, and the yield was 95.1%.

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Abstract

The purpose of this invention is to provide a kind of 3-hydroxyl-4-nitrobenzoic acid and preparation method thereof, take cheap and easy-to-get m-cresol as raw material, first nitration reaction, then carry out oxidation reaction. with H 2 o 2 As an oxidizing agent, the methyl group is oxidized to a carboxyl group, thereby producing 3-hydroxyl-4-nitrobenzoic acid. The method has the advantages of low raw material cost, simple operation, few by-products, high yield, mild reaction environment conditions, and is suitable for large-scale industrial production.

Description

Technical field: [0001] The invention relates to the technical field of biomedicine, in particular to 3-hydroxy-4-nitrobenzoic acid and a preparation method thereof. Background technique: [0002] p-Nitrobenzoic acid is an important intermediate in the fine organic product industry and the pharmaceutical industry. It can be used as a raw material to further prepare many important medicines or fine organic products. It is used in the production of procaine drugs, folic acid, benzocaine, and some drugs for the treatment of high blood pressure, and it is also an essential raw material for indole esters that regulate plant growth. Among them, the 3-substituted p-nitrobenzoic acid derivative is also an important pharmaceutical intermediate, and the industrial demand is also large, and the research on its preparation method has also received extensive attention. [0003] Wherein the preparation method of 3-hydroxyl-4-nitrobenzoic acid is seldom introduced in domestic patents. Ch...

Claims

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Application Information

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IPC IPC(8): C07C205/59C07C201/12
CPCC07C201/12C07C201/08C07C205/59C07C205/22
Inventor 叶芳
Owner 叶芳
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