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Synthesis method of 2-amino-5-fluorobenzoicacid methyl ester

A technology of methyl fluorobenzoate and a synthesis method, applied in the synthesis field of methyl 2-amino-5-fluorobenzoate, can solve the problems that cannot be used for synthesizing methyl 2-amino-5-fluorobenzoate and the like, Achieve the effect of improving catalytic activity and stability, increasing yield and product purity, and increasing specific surface area

Active Publication Date: 2017-01-25
泰州祥泰康华医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method cannot be used for the synthesis of methyl 2-amino-5-fluorobenzoate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Methyl 2-amino-5-fluorobenzoate was synthesized according to the following steps:

[0027] (1) Add tapioca starch to distilled water, the mass ratio of tapioca starch to distilled water is 1:5, heat to 90°C and reflux for 2 hours to obtain a fully dissolved starch mixture, and place the starch mixture in the lining material as polystyrene In an autoclave made of vinyl fluoride, put the autoclave into an oven, react at 160°C for 10 hours, take it out after naturally cooling to room temperature, wash repeatedly with deionized water and absolute ethanol, and vacuum dry at 90°C for 9 hours to obtain tapioca-based toner;

[0028] (2) Add the tapioca starch-based carbon powder obtained in step (1) into a muffle furnace, heat up to 600°C under a nitrogen atmosphere, and then roast for 4 hours to obtain tapioca starch-based carbon spheres. Add tapioca starch-based carbon spheres to hydrogen peroxide, and tapioca The mass ratio of starch-based carbon spheres to hydrogen peroxid...

Embodiment 2

[0033] Methyl 2-amino-5-fluorobenzoate was synthesized according to the following steps:

[0034] (1) Add tapioca starch to distilled water, the mass ratio of tapioca starch to distilled water is 1:6, heat to 90°C and reflux for 2 hours to obtain a fully dissolved starch mixture, and place the starch mixture in the lining material as polystyrene In an autoclave made of vinyl fluoride, put the autoclave into an oven, react at 160°C for 10 hours, take it out after naturally cooling to room temperature, wash repeatedly with deionized water and absolute ethanol, and vacuum dry at 90°C for 9 hours to obtain tapioca-based toner;

[0035] (2) Add the tapioca starch-based carbon powder obtained in step (1) into a muffle furnace, heat up to 600°C under a nitrogen atmosphere, and then roast for 4 hours to obtain tapioca starch-based carbon spheres. Add tapioca starch-based carbon spheres to hydrogen peroxide, and tapioca The mass ratio of starch-based carbon spheres to hydrogen peroxid...

Embodiment 3

[0040] Methyl 2-amino-5-fluorobenzoate was synthesized according to the following steps:

[0041] (1) Add tapioca starch to distilled water, the mass ratio of tapioca starch to distilled water is 1:7, heat to 90°C and reflux for 2 hours to obtain a fully dissolved starch mixture, and place the starch mixture in the lining material as polystyrene In an autoclave made of vinyl fluoride, put the autoclave into an oven, react at 160°C for 10 hours, take it out after naturally cooling to room temperature, wash repeatedly with deionized water and absolute ethanol, and vacuum dry at 90°C for 9 hours to obtain tapioca-based toner;

[0042] (2) Add the tapioca starch-based carbon powder obtained in step (1) into a muffle furnace, heat up to 600°C under a nitrogen atmosphere, and then roast for 4 hours to obtain tapioca starch-based carbon spheres. Add tapioca starch-based carbon spheres to hydrogen peroxide, and tapioca The mass ratio of starch-based carbon spheres to hydrogen peroxid...

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PUM

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Abstract

The invention provides a synthesis method of 2-amino-5-fluorobenzoicacid methyl ester. The synthesis method includes the steps of (1), preparing cassava starch-based carbon powder from cassava starch through a hydrothermal method; (2), preparing cassava starch-based carbon balls from the cassava starch-based carbon powder by means of roasting and then subjecting the cassava starch-based carbon balls to treatment of hydrogen peroxide so as to obtain oxidized cassava starch-based carbon balls; (3), mixing phosphotungstic acid with the oxidized cassava starch-based carbon balls so as to obtain a phosphotungstic acid compound catalyst; (4), subjecting 3-fluorobenzoic acid to nitration so as to obtain 5-fluoro-2-nitrobenzoic acid; (5), subjecting the 5-fluoro-2-nitrobenzoic acid and methyl alcohol to esterification reaction through the phosphotungstic acid compound catalyst so as to obtain methyl 5-fluoro-2-nitrobenzoate; (6) subjecting the methyl 5-fluoro-2-nitrobenzoate to reduction of palladium on carbon so as to obtain the 2-amino-5-fluorobenzoicacid methyl ester. The synthesis method has the advantages of high product yield and high product purity.

Description

technical field [0001] The invention relates to the field of pharmaceutical intermediates, in particular to a synthetic method of 2-amino-5-fluorobenzoic acid methyl ester. Background technique [0002] Fluorine-containing 2-aminobenzoic acid and methyl 2-aminobenzoate are important organic chemical intermediates, widely used in the fields of medicine, pesticides and fine chemicals. The synthetic method used in China is generally: (1) use 3-fluorobenzoic acid as raw material, utilize thionyl chloride to carry out acylation reaction; (2) carry out esterification reaction with methanol, obtain 3-fluorobenzoic acid methyl ester; (3) Nitration reaction of methyl 3-fluorobenzoate and mixed acid to obtain methyl 2-nitro-5-fluorobenzoate; (4) low-pressure reduction with palladium on carbon to obtain the target product. The total yield of this synthetic method is about 40%, which is not ideal enough and is not conducive to realizing large-scale production. [0003] The Chinese pat...

Claims

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Application Information

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IPC IPC(8): C07C227/04C07C229/56C07C201/12C07C205/58B01J31/18B01J27/188
CPCB01J27/188C07C201/08C07C201/12C07C227/04C07C205/58C07C229/56
Inventor 叶芳
Owner 泰州祥泰康华医药科技有限公司