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Preparation technology of phenyl boronic acid

A preparation process, the technology of phenylboronic acid, which is applied in the field of pharmaceutical intermediates, can solve the problems of difficult separation, low product yield and high cost of phenylboronic acid, and achieve the effect of reducing production cost and saving raw materials

Inactive Publication Date: 2006-01-11
何连岐
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the trimethyl borate itself is unstable, the product yield of phenylboronic acid is very low, generally only 40% yield is good, and because the trimethyl borate decomposes to generate methanol, which is similar in nature to tetrahydrofuran , is not easy to separate, and causes great difficulties to solvent recycling. Due to this factor, the cost of the product remains high (up to about 2000 yuan / ton)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Preparation of the first step Grignard reaction solution

[0016] In 50 liters of reactors, add 20 liters of water and be less than 0.1% tetrahydrofuran, 6 kilograms of magnesium bars, 0.5 kilograms of bromobenzene and 100 milliliters of prepared phenylmagnesium bromide to initiate the reaction, after the reaction is initiated, Control the temperature at 30-35 degrees, add dropwise a solution of 15 liters of tetrahydrofuran and 13 kg of bromobenzene, and keep it warm for 1 hour to obtain the Grignard reaction solution.

[0017] Preparation of the second step phenylboronic acid

[0018] Add 30 liters of tetrahydrofuran and 30 kg of tributyl borate into a 100-liter kettle, lower the temperature to minus 60°C, add the reaction solution prepared above dropwise, and keep the temperature for 30 minutes after the addition; then add 10% hydrochloric acid to react to form butanol and To acidic, PH is controlled at 2, and the addition is completed. Naturally raise the temperatu...

Embodiment 2

[0020] In the preparation process of the above-mentioned second step of phenylboronic acid, 10% hydrochloric acid is added dropwise to form butanol and become acidic, and the pH can be controlled at 1.

[0021] The cost of phenylboronic acid produced by the above process can be controlled below 700 yuan / ton.

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Abstract

A process for preparing phenylboric acid includes two steps: preparing Grig nard reaction liquid and preparing phenylboric acid. In the second step, the tributyl borate is used to replace trimethyl borate, resulting in high output rate (more than 60%) and low cost.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical intermediates, in particular to a preparation method of phenylboronic acid. Background technique [0002] The pharmaceutical industry is a sunrise industry in today's chemical industry. More and more new drug production depends on the production of some key intermediate raw materials. Only when the supply of pharmaceutical intermediates meets the demand can the drug cost be greatly reduced and the drug more efficient. Good service for the health of the people. Phenylboronic acid is one such intermediate product. [0003] Phenylboronic acid was first discovered by the Japanese and its reaction mechanism was studied. In-depth theory and practice show that the appearance of phenylboronic acid will bring about a revolution in the chemical synthesis industry. As we all know, the coupling of benzene rings is very difficult in chemical production. The old methods general...

Claims

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Application Information

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IPC IPC(8): C07F5/02
Inventor 何连岐
Owner 何连岐
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