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Purification method of organic boric acid compound

A technology of organic boric acid and purification method, which is applied in the direction of organic chemistry, chemical instruments and methods, and compounds containing elements of group 3/13 of the periodic table, etc. It can solve the problems of high content of inorganic boric acid, affecting accurate quantitative feeding, etc., and achieve operational easy effect

Active Publication Date: 2016-06-15
CANGZHOU PURUI DONGFANG SCI & TECH
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  • Summary
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Problems solved by technology

In the organic boric acid obtained by these two methods, there are too high content of inorganic boric acid, unreacted dehalogenated by-products, and the coexistence of trimer and monomer, which directly affect the subsequent use in coupling reactions. Accurate quantitative feeding, as well as product preservation and stability

Method used

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  • Purification method of organic boric acid compound

Examples

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Comparison scheme
Effect test

Embodiment 1

[0017] Purification of isobutylboronic acid:

[0018] In a 500 ml single-necked bottle, add 60 grams of solid crude isobutylboronic acid obtained by isobutyl Grignard reagent and trimethyl borate (the pinacol derivatization method measures GC: 94.6%) and 35 ml of absolute ethanol, and stir at room temperature After 10-20 minutes, dissolve completely, and then slowly add 180 ml of water dropwise. After the dropwise addition, continue to stir until the solid precipitates completely, filter, wash the filter cake with 15 ml of water, and dry it in a vacuum oven to obtain a scaly solid isobutyl 52 grams of base boronic acid, GC: 99.2% determined by derivatization method, no inorganic boronic acid peak was detected by HNMR, water content determined by Karl Fischer: 35.11% (theoretical value: 35.35%).

Embodiment 2

[0020] Purification of cyclopropylboronic acid:

[0021] In a 500 ml single-necked bottle, add 60 grams of crude product cyclopropylboronic acid (GC: 96.3% by neopentyl glycol derivatization method) and 30 ml of anhydrous methanol obtained by adding the solid-liquid mixture obtained by cyclopropyl Grignard reagent and trimethyl borate After stirring at room temperature for 10-15 minutes, dissolve completely, and then slowly add 210 ml of 2% hydrochloric acid aqueous solution dropwise. Obtained 56 grams of scaly solid cyclopropylboronic acid, GC: 99.6% determined by derivatization method, no inorganic boric acid peak was detected by HNMR, water content determined by Karl Fischer: 42.05% (theoretical value: 41.96%).

Embodiment 3

[0023] Purification of phenylboronic acid:

[0024] In a 500 ml single-necked bottle, add 50 grams of crude product phenylboronic acid (HPLC: 96.5%) and 25 ml of anhydrous methanol to the solid-liquid mixture obtained by adding phenyl Grignard reagent and trimethyl borate, and stir at room temperature for 10-15 minutes. Dissolve and clear, and then slowly add 150 ml of 2% hydrochloric acid aqueous solution dropwise. After the dropwise addition, continue to stir until the solid precipitates completely, filter, wash the filter cake with 20 ml of water, and obtain 45 grams of fine needle-shaped solid phenylboronic acid after vacuum drying. HPLC : 99.8%, HNMR detection of inorganic boric acid content of 0.1%, Karl Fischer determination of water: 29.10% (theoretical value: 29.56%).

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Abstract

The invention provides a purification method of an organic boric acid compound. The method includes: adding an alcohol solvent into an organic boric acid compound crude product obtained by Grignard or lithiation method till complete dissolution, then adding excess water or acid water solution to precipitate solid again, and conducting filtering and drying so as to obtain a boric acid pure product. The method provided by the invention can remove unreacted dehalogenation by-product, inorganic boric acid and other main impurities from the organic boric acid crude product to obtain organic boric acid with purity of more than 99%.

Description

technical field [0001] The invention relates to a method for purifying organic boric acid compounds, which belongs to the field of fine chemical intermediates. Background technique [0002] In recent years, the industrial application of organic boric acid has been increasing year by year. Since the high-efficiency reaction can be realized under mild conditions, after Suzuki coupling won the Nobel Prize in 2010, organic boronic acid, as one of the main raw materials for this coupling reaction, has developed rapidly in the fields of medicine and OLED materials. [0003] The synthesis of organoboronic acid mainly adopts Grignard method and lithiation method at present. The Grignard method uses a halide to make a Grignard reagent, then reacts with trimethyl borate, hydrolyzes it, extracts it with ethyl acetate, and distills it to make a slurry; the lithiation method uses a halide to exchange lithium with metal lithium or n-butyllithium. Afterwards, react with triisopropyl bora...

Claims

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Application Information

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IPC IPC(8): C07F5/02
CPCC07F5/025
Inventor 冷延国桂迁张进
Owner CANGZHOU PURUI DONGFANG SCI & TECH
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