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Preparation method of 1-fluorin-6-iodo-benzoic acid

A technology of iodobenzoic acid and methyl iodobenzoate is applied in directions such as carboxylate/lactone preparation, organic chemistry, etc., and can solve problems such as unfavorable industrialized production, high production cost, harsh conditions and the like

Inactive Publication Date: 2012-07-04
SHANGHAI SINOFLUORO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing technology needs to react at low temperature, the conditions of this kind of reaction are relatively harsh, and the production cost is high, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Pour 350ml of methanol and 164.2g (0.59mol) of the above crude 1-fluoro-6-iodobenzoic acid methyl ester into a 1L four-necked bottle under stirring, and add dropwise the product formed by dissolving 35g (0.9mol) in 200ml of water after stirring. Keep the reaction temperature at 40 to 50 degrees Celsius, follow up and detect until the raw materials have reacted completely, and precipitate a yellow granular solid after being acidified with dilute hydrochloric acid, wash with water, dissolve with 5% sodium hydroxide aqueous solution, and decolorize the active carbon after alkali dissolution, acid analysis, cooling, Crystallized and dried to obtain 145.0 g of white crystals with a content of 99.82% (detected by liquid chromatography) and a yield of 54.51%.

Embodiment 2

[0012] Pour 250ml of methanol and 64.2g of the above crude 1-fluoro-6-iodobenzoate methyl ester into a 1L four-necked bottle with stirring, and add dropwise the solution formed by dissolving 25g in 200ml of water after stirring to keep the reaction temperature at 40 To 50 degrees Celsius, follow up and detect until the reaction of the raw materials is complete, acidify with dilute hydrochloric acid, precipitate a yellow granular solid, wash with water, dissolve with 5% sodium hydroxide aqueous solution, decolorize the activated carbon, acidify, cool, crystallize, and dry to obtain 45.0g white Crystal content 98.82% (detected by liquid chromatography), yield 53.51%.

Embodiment 3

[0014] Pour 150ml of methanol and 14.2g of the above crude 1-fluoro-6-iodobenzoate methyl ester into a 1L four-necked bottle with stirring, and add dropwise the solution formed by dissolving 15g in 200ml of water after stirring to keep the reaction temperature at 40 To 50 degrees Celsius, follow up and detect until the raw materials are completely reacted, acidify with dilute hydrochloric acid, precipitate a yellow granular solid, wash with water, dissolve with 5% sodium hydroxide aqueous solution, decolorize activated carbon, acidify, cool, crystallize, and dry to obtain 15.0g white Crystal content 97.62% (detected by liquid chromatography), yield 52.71%.

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PUM

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Abstract

The invention provides a preparation method of 1-fluorin-6-iodo-benzoic acid. The 1-fluorin-6-iodo-benzoic acid is synthesized by taking 1-fluorin-6-iodo-methyl formate as a raw material and taking methanol as a solvent. The method has the advantages of reaction operability, easiness, practicability and industrial production application value.

Description

technical field [0001] The invention relates to the field of fluorine chemical industry, in particular to a synthesis method of 1-fluoro-6-iodobenzoic acid. Background technique [0002] 1-Fluoro-6-iodobenzoic acid is an intermediate of pesticides and medicines, and a drug intermediate of bradykinin receptor antagonists. It can also synthesize drugs that can inhibit the side effects of certain anti-tumor drugs. Pharmaceutical intermediates of kinin receptor antagonists. The prior art needs to react at low temperature, the conditions of this type of reaction are relatively harsh, the production cost is high, and it is not conducive to industrial production. Contents of the invention [0003] The object of the present invention is to provide a method for the catalytic synthesis of 1-fluoro-6-iodobenzoic acid starting from readily available reagents. A preparation method of 1-fluoro-6-iodobenzoic acid has been found, using methyl 1-fluoro-6-iodobenzoate as a raw material an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/70C07C51/09
Inventor 张巍江静
Owner SHANGHAI SINOFLUORO SCI
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