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Bis(pinacolato)diboron production process

A kind of biboronic acid pinacol ester, the technology of production technology, applied in the field of biboronic acid pinacol ester production technology, can solve the problems of waste of resources, low reaction conversion rate, low product yield, etc., to avoid extremely low temperature conditions, Effects of improving safety and improving reaction conversion rate

Active Publication Date: 2012-07-11
HAIMEN RUIYI MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Pinacolate diborate is a pharmaceutical intermediate, its English alias: bis (pinacolato) diboron, molecular formula is C12H24B2O4, the existing production process of pinacolate borate is not safe, and the reaction conversion rate is low , the product yield is low, resulting in waste of resources

Method used

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  • Bis(pinacolato)diboron production process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The production technology of pinacol ester of diboronic acid comprises the steps:

[0017] (1) First, add 1900 parts by volume of n-hexane with a mass concentration of 97% into a four-necked bottle equipped with a mechanical stirrer, a thermometer, an exhaust gas absorption device and a condenser tube, and stir, then introduce 180 parts by mass of boron trichloride gas , under the condition of 10°C and normal pressure, 470 parts by mass of dimethylamine gas was introduced to carry out the amination reaction, and then the precipitated salt was removed by suction filtration, and the filtrate was re-added into the four-necked bottle;

[0018] (2) Add 210 parts by mass of boron tribromide dropwise to the above filtrate within 55 minutes, and react for 4.5 hours at normal temperature and pressure. Distill to obtain n-hexane first, then reduce the pressure to -0.09MPa, cool down to 60°C to distill the intermediate;

[0019] (3) Take another four-necked bottle, add 2900 parts...

Embodiment 2

[0022] The production technology of pinacol ester of diboronic acid comprises the steps:

[0023] (1) First add 2000 parts by volume of n-hexane with a mass concentration of 98% into a four-neck bottle equipped with a mechanical stirrer, a thermometer, an exhaust gas absorption device and a condenser tube, and stir, then feed 200 parts by mass of boron trichloride gas , under the condition of 12°C and normal pressure, 480 parts by mass of dimethylamine gas was introduced to carry out the amination reaction, and then the precipitated salt was removed by suction filtration, and the filtrate was re-added into the four-necked bottle;

[0024] (2) Add 220 parts by mass of boron tribromide dropwise to the above filtrate within 60 minutes, and react for 5 hours at normal temperature and pressure. Distill to obtain n-hexane first, then reduce the pressure to -0.095MPa, cool down to 62°C to distill the intermediate;

[0025] (3) Take another four-necked bottle, add 3000 parts by volum...

Embodiment 3

[0028] The production technology of pinacol ester of diboronic acid comprises the steps:

[0029] (1) First add 2100 parts by volume of n-hexane with a mass concentration of 99% into a four-necked bottle equipped with a mechanical stirrer, a thermometer, an exhaust gas absorption device and a condenser tube, and stir, then feed 210 parts by mass of boron trichloride gas , under the condition of 15°C and normal pressure, 490 parts by mass of dimethylamine gas was introduced to carry out the amination reaction, and then the precipitated salt was removed by suction filtration, and the filtrate was re-added into the four-necked bottle;

[0030] (2) Add 230 parts by mass of boron tribromide dropwise to the above filtrate within 65 minutes, and react for 5.5 hours at normal temperature and pressure. First distill to obtain n-hexane, then reduce the pressure to -0.1MPa, cool down to 65°C to distill the intermediate;

[0031] (3) Take another four-necked bottle, add 3100 parts by vol...

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Abstract

The invention discloses a bis(pinacolato)diboron production process which is characterized in that boron trichloride is used as a raw material and is aminated with dimethylamine gas in an n-hexane system, the desalinated reaction solution and boron tribromide react at the room temperature, the prepared intermediate and magnesium are coupled in toluene, 1, 2-dichloroethane solution of pinacol is dropped into the desalinated reaction solution, and the target product is prepared via transesterification. The invention has the advantages that: n-hexane is used as a reaction solvent for the first two steps, the conversion rate of reaction is increased, and the ultra low temperature can be avoided; the safety of the process is improved due to use of magnesium; and the yield of the product is increased in transesterification through controlling the reaction temperature.

Description

technical field [0001] The invention relates to a production process of biboronic acid pinacol ester. Background technique [0002] Pinacolate diborate is a pharmaceutical intermediate, its English alias: bis (pinacolato) diboron, molecular formula is C12H24B2O4, the existing production process of pinacolate borate is not safe, and the reaction conversion rate is low , the product yield is low, resulting in waste of resources. Therefore, a new technical solution should be provided to solve the above problems. Contents of the invention [0003] The object of the invention is: aim at above-mentioned deficiency, provide a kind of production technique of the pinacol ester of diboronic acid high in process safety, reaction conversion rate high, product yield high. [0004] In order to achieve the above object, the technical scheme adopted in the present invention is: [0005] The production technology of pinacol ester of diboronic acid comprises the steps: [0006] (1) Firs...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/04
Inventor 薛嵩
Owner HAIMEN RUIYI MEDICAL TECH
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