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The preparation method of oxidizing agent ibx

A high-boiling-point solvent and iodobenzoic acid technology, applied in organic chemistry and other fields, can solve problems such as personal casualties, low purity of potassium persulfate oxidation, and regional pollution

Active Publication Date: 2020-03-27
SHANGHAI ZAIQI BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Among the above four methods, potassium permanganate may cause heavy metal pollution; potassium bromate is a carcinogen and bromine vapor will be released during the reaction, which is very inconvenient to operate and has the risk of environmental pollution; chlorine gas is poisonous, and chlorine gas leakage is extremely serious. It is easy to cause personal casualties and regional pollution; the oxidation purity of potassium hydrogen persulfate is not high

Method used

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  • The preparation method of oxidizing agent ibx
  • The preparation method of oxidizing agent ibx
  • The preparation method of oxidizing agent ibx

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 2-Iodobenzoic acid (50.0 g, 0.20 mol) was added to sulfolane (250 mL), and the solution was heated to 50°C. 90% of the above solution was slowly added dropwise to an aqueous solution (300 mL) of potassium hydrogen persulfate (147.4 g, 0.24 mol, 1.2 equiv) at 50°C, and the reaction was incubated for 3 hours. Then the reaction solution was heated to 95° C. and the remaining 10% 2-iodobenzoic acid solution was slowly added dropwise to the reaction solution, and the reaction was continued for 3 hours. After the reaction was complete, it was cooled to 5°C and stirring was continued at this temperature for 1.5 hours. Add 1L of water under stirring, filter (the filtrate is to be recycled), the filter cake is rinsed with water and acetone successively, and dried at room temperature for 16 hours to obtain 53.2 g of white solid (yield 95.04%), and the purity of IBX is 99.7% (confirmed by NMR and HPLC ). The solid was determined to be IBX by HNMR detection. H NMR (400MHz, DMSO-...

Embodiment 2

[0028] 2-Iodobenzoic acid (5kg, 20mol) was added to DMF (25L), and the solution was heated to 60°C. 85% of the above solution was slowly added dropwise to an aqueous solution (40 L) of potassium hydrogen persulfate (22.1 kg, 36 mol, 1.8 equiv) at 60°C, and the reaction was incubated for 3 hours. The reaction was heated to 95° C. and the remaining 15% 2-iodobenzoic acid solution was slowly added dropwise to the reaction liquid, and the reaction was continued for 2 hours. After the reaction was complete it was cooled to 0°C and stirring was continued at this temperature for 1 hour. 100L of water was added under stirring, and after filtration, the filter cake was rinsed with water and acetone successively and dried at room temperature for 16 hours to obtain 4.51kg (yield 80.53%) of a white solid, and the purity of IBX was 99.8% (confirmed by NMR and HPLC). The standard spectrum is consistent.

Embodiment 3

[0030] 2-Iodobenzoic acid (50kg, 200mol) was added to dimethylsulfoxide (250L), and the solution was heated to 55°C. 90% of the above solution was slowly added dropwise to an aqueous solution (300 L) of potassium hydrogen persulfate (159.6 kg, 260 mol, 1.3 equiv) at 70°C. React at 70°C for 3 hours. The reaction was heated to 90° C., and the remaining 10% 2-iodobenzoic acid solution was slowly added dropwise to the reaction liquid, and the reaction was continued for 3 hours. After the reaction was complete it was cooled to 0°C and stirring was continued at this temperature for 2 hours. 1000L of water was added under stirring, and the filtered cake was rinsed with water and acetone successively and dried at room temperature for 16 hours to obtain 45.4kg of white solid (yield 81.07%). The purity of IBX was 99.8% (confirmed by NMR and HPLC). NMR and standard The spectra are consistent.

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Abstract

The invention discloses a preparation method of 2-iodoxy benzoic acid. The preparation method includes: 2-iodobenzoic acid, potassium hydrogen sulfate and the like are used as the raw materials to prepare the product 2-iodoxy benzoic acid through one-step reaction. The preparation method has the advantages that the preparation method is simple and stable in process operation, easy in product separation and high in yield, and product purity reaches 99.5% or above; the raw materials are cheap and easy to obtain, the production cost of existing biological, medicinal and chemical intermediates islowered greatly, and industrial large-scale production is benefited.

Description

technical field [0001] The invention belongs to the field of pharmaceutical chemical synthesis, and in particular relates to a preparation method of an oxidant IBX. Background technique [0002] IBX is the abbreviation of 2-Iodoxybenzoic acid, the molecular formula is C 7 h 5 IO 4 . IBX is white crystal, melting point: 232-233°C, easily soluble in DMSO, but almost insoluble in general organic solvents. IBX is easy to prepare, non-toxic, and stable to water and air. The reactivity is unique. High selectivity, relatively mild reaction conditions, high yield, is an ideal oxidant. [0003] The preparation of IBX generally all is to use o-iodobenzoic acid as a raw material, and is oxidized with various oxidizing agents, and the reaction is as follows: [0004] [0005] Depending on the oxidant used, there are several methods: Potassium permanganate, potassium bromate, chlorine gas, and potassium persulfate oxidation. [0006] Among the above four methods, potassium per...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D347/00
CPCC07D347/00
Inventor 李开孙鹏李超田贝贝
Owner SHANGHAI ZAIQI BIO TECH