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A kind of synthetic boron amine compound technology and product application

A compound and boron amine technology, applied in the new process of synthesizing boron amine compounds and product application fields, can solve the problems of heavy metal residues and high cost of boronate esters, improve product yield and purity, reduce operating equipment, and avoid ultra-low temperature reactions. Effect

Active Publication Date: 2018-10-30
CANGZHOU PURUI DONGFANG SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are disadvantages such as high cost and easy heavy metal residues in the preparation of borate by coupling reaction

Method used

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  • A kind of synthetic boron amine compound technology and product application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Compound MeB(N i -Pr 2 ) 2 Synthesis:

[0020] Under nitrogen protection, in a three-necked flask equipped with a dropping device, add magnesium metal (0.11 mol) and 10 ml of tetrahydrofuran, cool down to 0°C, and start to add methyl iodide (0.1 mol) and bis(N,N-diiso) propyl)boron bromide (0.11 mol) was dissolved in 150 mL of tetrahydrofuran. After 15-20 ml was added dropwise, stirring was continued for about 10-20 minutes, and the temperature of the reaction solution rose from 0°C to 6°C, which indicated that the reaction had been initiated. After the addition was completed, the temperature was naturally raised to room temperature and the reaction was continued for 3-5 hours with stirring, and GC confirmed the completion of the reaction. Saturated ammonium chloride was added for quenching, and the pH value of the solution was adjusted to 4-5. After adding ethyl acetate, the layers were separated, the aqueous layer was extracted once more with ethyl acetate, and t...

Embodiment 2

[0022] Compound CH 2 =CHCH 2 B(N i -Pr 2 ) 2 Synthesis:

[0023] Under nitrogen protection, in the there-necked flask equipped with dripping and reflux device, add magnesium metal (0.12 mole), 15 ml of 2-methyltetrahydrofuran and several small grains of iodine, be warming up to 50 ℃, start to drip allyl chloride ( 0.1 mol) and bis(N,N-diisopropyl)boron bromide (0.1 mol) were dissolved in 110 mL of 2-methyltetrahydrofuran solution. After the initial dropwise addition of 15-20 ml, the stirring was continued for about 10-20 minutes, and the purple color in the reaction solution disappeared, indicating that the reaction had been initiated. After the addition was completed, the temperature was maintained and the stirring reaction continued for 3-5 hours, and GC confirmed the completion of the reaction. Saturated ammonium chloride was added for quenching, and the pH value of the solution was adjusted to 4-5. The layers were separated, the aqueous layer was extracted once more...

Embodiment 3

[0025] compound Synthesis:

[0026] Under nitrogen protection, in a three-necked flask equipped with a dripping and reflux device, add metallic magnesium (0.11 mol), 10 milliliters of tetrahydrofuran and a few small grains of iodine, be warming up to 50 ° C, and begin to drip cyclopropyl bromide (0.1 mol) and Bis(tetrahydropyrrole)boron bromide (0.1 mol) was dissolved in 130 mL of tetrahydrofuran solution. After the initial dropwise addition of 15-20 ml, continue stirring for about 5-10 minutes, and the purple color in the reaction solution disappears, indicating that the reaction has been initiated. After the addition was completed, the temperature was raised to reflux and the stirring was continued for 3-5 hours. GC confirmed that the reaction was completed. After cooling, add saturated ammonium chloride to quench, and adjust the pH value of the solution to 4-5. After adding ethyl acetate, the layers were separated, the aqueous layer was extracted once more with ethyl ac...

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Abstract

The invention discloses a boron amine compound synthesis technology and product application. Halogenate RX, halogenate BrBY2 and solvent are mixed and added into initiator and magnesium metal in a dropwise mode, and the temperature is kept within the range from 0 DEG C to 80 DEG C in the dropping process; after a reaction occurs, the rest is added, then the temperature is kept within the range from 20 DEG C to 80 DEG C for the reaction, saturation ammonium chloride is added for quenching, and after reduced pressure distillation, RBY2 is obtained. The technology is simple in operation, ultrlow temperature conditions, Grignard reagent concentration and the self-coupling problem are avoided, the reaction yield is high, the product stability is good, and the technology is suitable for being popularized in an industrialization mode. After the product is subjected to a derivatization reaction with KHF2 and MIDA, RBF3K and RB (MIDA) can be obtained.

Description

technical field [0001] The invention relates to a new process and product application for synthesizing boron amine compounds, and belongs to the field of fine chemical intermediates. Background technique [0002] In recent years, as people pay more and more attention to health, and the pace of corresponding new drug research and development is getting faster and faster, various organic chemical reactions are emerging one after another. As the most direct, effective and mild way to construct carbon-carbon bonds, the Suzuki coupling reaction is naturally favored by the industry and has been successfully used in the synthesis of many new drugs that have been marketed. [0003] As an important raw material for Suzuki coupling, the synthesis of boronic acid / ester is currently mainly in the following two ways: a Grignard reagent involving metal magnesium or a lithium reagent involving metal lithium / alkyllithium reacts with trimethyl borate, and then reacts with trimethyl borate af...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/02
Inventor 冷延国桂迁张进
Owner CANGZHOU PURUI DONGFANG SCI & TECH
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