Preparation method of o-iodobenzoic acid

A technology of benzoic acid and o-iodine, which is applied in the field of pharmaceutical synthesis chemistry, can solve problems such as long approval time, high production cost, and production impact, and achieve the effects of unaffected production and operation, convenient production and purchase, and high safety and stability

Inactive Publication Date: 2021-01-15
苏州华鑫医药科技有限公司
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Problems solved by technology

[0004] However, for the preparation of the starting material o-iodobenzoic acid of the Dess-Mating oxidation reagent, an industrial route is to use anthranilic acid as a raw material, diazotize to obtain o-iodobenzoic acid, and then recrystallize and refine to obtain o-iodobenzoic acid Benzoic acid, see figure 1 , because anthranilic acid is listed as a controlled product in the catalog of the "Regulations on the Administration of Precursor Chemicals", it is controlled by the public security department and managed by the "Regulations on the Safety Management of Hazardous Chemicals". It is very inconvenient to produce and purchase, and the approval time Long, the approval amount is limited, and the production is often affected; the price of anthranilic acid is relatively expensive, and the production cost is high; the safety risk of anthranilic acid is relatively high

Method used

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  • Preparation method of o-iodobenzoic acid
  • Preparation method of o-iodobenzoic acid

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Embodiment Construction

[0029] The present invention will be further described below in conjunction with specific embodiments and drawings.

[0030] The specific technical scheme is as follows:

[0031] Add 130-145kg of sodium nitrite powder to 40-50kg of water to form a clear solution; add 1400-1500g of water to the reaction flask, then slowly add 250-270kg of concentrated sulfuric acid solution into the reaction flask, and stir evenly to obtain Diluted sulfuric acid solution; finally, add 270-280kg of methyl anthranilate liquid into the diluted sulfuric acid solution, stir and cool down to below 0°C, add the pre-configured sodium nitrite aqueous solution dropwise, and control the The reaction temperature is not higher than 5°C. When the solution gradually becomes clear during the dropping process, and the color changes from red to yellow, the dropping is completed. After the dropping is completed, keep warm for 2 hours and store at low temperature for later use; add 600-650kg of water, Heat 4-5kg ...

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Abstract

The invention relates to a preparation method of o-iodobenzoic acid. According to the invention, methyl anthranilate is used as an initial raw material instead of anthranilic acid, so that the management of I type easily-prepared toxic raw materials of anthranilic acid is avoided; and according to product properties, methyl o-iodobenzoate is purified in a distillation manner by using a new purification method, so that the purity is high, and the safety is high.

Description

technical field [0001] The invention relates to the field of pharmaceutical synthetic chemistry, in particular to a new process route for synthesizing o-iodobenzoic acid needed for synthesizing Dess-Mating oxides. Background technique [0002] In recent years, organic hypervalent iodine compounds have been widely used in important fields of organic synthesis due to their easy preparation, mild performance, high selectivity and environmental friendliness. Dess-Mating oxidation reagent is one of the organic hypervalent iodine compounds. Dess-Mating oxidation Reagent is the most researched and most widely used. Dess-Mating oxidizing reagent (also known as Dess-Martin oxidizing agent) is a commonly used, mild and selective oxidizing agent. [0003] At present, people often oxidize primary alcohols on Dess-Mating oxidation reagents to aldehydes, and secondary alcohols to ketones; it has the advantages of mild reaction conditions, moderate speed, less dosage, convenient post-treat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/31C07C69/76C07C51/09C07C27/02C07C63/70
CPCC07C51/09C07C67/31C07C69/76C07C63/70
Inventor 龙在华刘玲玲
Owner 苏州华鑫医药科技有限公司
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