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A kind of synthesis technique of tetrahydroxy diboron

A technology of tetrahydroxydiboron and synthesis process, which is applied to boron oxy compounds, boron oxyacids and other directions, 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: 2019-06-18
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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  • A kind of synthesis technique of tetrahydroxy diboron

Examples

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Effect test

Embodiment 1

[0020] In the reaction flask, after adding 10% hydrochloric acid (4.5eq), the temperature was lowered to 0°C, tetrakis(dimethylamino)biboron (39.6g, 0.2mol, 1.0eq) was slowly added dropwise to the above hydrochloric acid solution, and the During the process, solids were gradually precipitated out. After the dropwise addition, they were gradually raised to room temperature and stirred for 3 hours, filtered to obtain 16.9g after vacuum drying at 40-60°C, and the yield was 94.2%; GC derivation (dissolving the product in In methanol, adding pinacol derivative) detected 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 brackets are the peak area values}; add 60mL of 0.05% dilute hydrochloric acid to the above product, stir at a temperature of 5-10°C for 30 minutes, filter, and dry the obtained solid at 40-60°C to obtain 16.5g of a white product. GC-derived detection content 99.6%, HPLC: 99.9%; HNMR (DMSO-d6+H2O): 8.84 (0.0...

Embodiment 2

[0022] In the reaction flask, after adding 10% hydrochloric acid (5.5eq), the temperature was lowered to 10°C, tetrakis(dimethylamino)biboron (39.6g, 0.2mol, 1.0eq) was slowly added dropwise to the above hydrochloric acid solution, and the During the process, the temperature was controlled within 30°C, and solids were gradually precipitated out. After the dropwise addition was completed, the mixture was stirred at room temperature for 3 hours, filtered, and 16.2g was obtained after vacuum drying at 40-60°C to obtain a white solid product, with a yield of 90.4%; GC derivation ( The product is dissolved in methanol, and pinacol is added to derive) 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, tetrakis(dimethylamino)biboron (39.6g, 0.2mol, 1.0eq) was slowly added dropwise into the above nitric acid solution, and During the addition process, solids were gradually precipitated, and the temperature was controlled within 0°C. After the dropwise addition was completed, it was gradually raised to room temperature and stirred for 3 hours, filtered, and a white solid product was obtained. After vacuum drying at 40-60°C, 16.7g was obtained, with a yield of 93.3%. ; GC derivation (dissolving the product in methanol, adding pinacol derivatization) detected 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 tetrahydroxy diboron, which belongs to the field of synthesis of pharmaceutical intermediates. Background technique [0002] Tetrahydroxydiboron, also known as diboronic acid, diboronic acid or biboronic acid, English name: Tetrahydroxydiboron or Bis-boronic acid, CAS: 13675-18-8, English abbreviation BBA, mainly used in Suzuki coupling Chinese synthetic medicine intermediate. [0003] At present, there are few literature reports on the synthesis method, but the application examples have been increasing 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 academia and industry are showing the trend of replacing the above reagents. [0004] Judging from the only few documents, the earliest synthesis of tetrahydroxydiboron can be traced back to 1955. Wartik used a zinc electrode inserte...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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