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Synthesis technology of tetrahydroxy diboron

A technique for the synthesis of tetrahydroxydiboron, which is applied in the direction of boron oxide compounds, boron oxyacids, etc., can solve problems such as large fluctuations in yield, and achieve the effects of safe and controllable process, obvious yield, and improved yield

Active Publication Date: 2018-05-22
CANGZHOU PURUI DONGFANG SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using the literature method, the method of adding tetrakis(dimethylamino) boron to hydrochloric acid dropwise, when verified on a large scale, the yield fluctuates greatly, and there is an obvious correlation between the dropping speed and temperature, and there is gas generation when the temperature rises simultaneously. Proven to be hydrogen, a potential safety hazard

Method used

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  • Synthesis technology of tetrahydroxy diboron

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In the reaction flask, after adding 10% hydrochloric acid (4.5eq), the temperature was lowered to 0°C, and tetrakis(dimethylamino)biboron (39.6g, 0.2mol, 1.0eq) was slowly added dropwise to the above hydrochloric acid solution, and added dropwise. During the process, there is gradually a solid precipitation, and the dropwise addition is completed, gradually rising to room temperature and stirring for 3 hours, filtering to obtain 16.9 g of a white solid product after vacuum drying at 40-60 ° C, a yield of 94.2%; GC derivatization (dissolving the product in In methanol, add pinacol derivatization) detection content 97.9%, HPLC: 99.5%; HNMR (DMSO-d6+H2O): 8.84 (0.02), 8.61 (1.00), 7.59 (5.28), 6.50 (0.02) {Note: The peak area value in brackets}; the above product was added with 60 mL of 0.05% dilute hydrochloric acid, stirred for 30 minutes under temperature control at 5-10 °C, filtered, and the obtained solid was dried at 40-60 °C to obtain 16.5 g of white product. Conten...

Embodiment 2

[0022] In the reaction flask, after adding 10% hydrochloric acid (5.5eq), the temperature was lowered to 10°C, and tetrakis(dimethylamino)biboron (39.6g, 0.2mol, 1.0eq) was slowly added dropwise to the above hydrochloric acid solution, and added dropwise. During the process, the temperature was controlled within 30°C, and a solid was gradually precipitated, and the dropwise addition was completed, stirring at room temperature for 3 hours, and filtering to obtain 16.2g of a white solid product after vacuum drying at 40-60°C, with a yield of 90.4%; GC derivatization ( Dissolve the product in methanol, add pinacol derivatization) detection content 97.3%, HPLC: 99.6%; HNMR (DMSO-d6+H2O): 8.84, 8.61, 7.59.

Embodiment 3

[0024] In the reaction flask, after adding 10% nitric acid (4.8eq), the temperature was lowered to -10°C, and tetrakis(dimethylamino)biboron (39.6g, 0.2mol, 1.0eq) was slowly added dropwise to the above nitric acid solution, dropwise During the adding process, gradually there is solid precipitation, the temperature is controlled within 0 ℃, the dropwise addition is completed, gradually rise to room temperature and keep stirring for 3 hours, filter to obtain 16.7g of white solid product after vacuum drying at 40-60 ℃, the yield is 93.3% ; GC derivatization (dissolve the product in methanol, add pinacol derivatization) detection content 97.3%, HPLC: 99.6%; HNMR (DMSO-d6+H2O): 8.84, 8.61, 7.59.

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Abstract

The invention discloses a synthesis technology of tetrahydroxy diboron. The synthesis technology comprises the following steps: with tetraalkylamine diboron as a raw material, adding into an excess aqueous acid solution, reacting, then filtering, and performing vacuum drying to obtain the tetrahydroxy diboron. By the synthesis technology, operation is simple, the yield is high, and the product purity and the content reach 97% or above; the synthesis technology is suitable for industrial scale-up production.

Description

technical field [0001] The invention relates to a synthesis process of tetrahydroxydiboron, and belongs to the field of synthesis of pharmaceutical intermediates. Background technique [0002] Tetrahydroxydiboron, also known as bis-diboronic acid, diboronic acid or bis-boronic acid, English name: Tetrahydroxydiboron or Bis-boronic acid, CAS: 13675-18-8, English abbreviation BBA, mainly used for Suzuki coupling Chinese synthesis medicine Intermediate. [0003] At present, there are few literature reports on the synthesis methods, but the application examples have increased year by year since 2010. , the by-product of the coupling reaction is inorganic boronic acid, and there are no by-products such as pinacol, neopentyl glycol or catechol. The academic and industrial circles are showing a trend of replacing the above reagents. [0004] From the few literatures, the earliest synthesis of tetrahydroxydiboron can be traced back to 1955. Wartik used the insertion of zinc electr...

Claims

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Application Information

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IPC IPC(8): C01B35/10
CPCC01B35/1045
Inventor 冷延国张进张朋岳
Owner CANGZHOU PURUI DONGFANG SCI & TECH
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