Preparation technology of phenylboronic acid reaction liquid

A technology of reaction solution and phenylboric acid, which is applied in the field of preparation technology of reaction solution, can solve the problems of complex preparation process of phenylboric acid and is not suitable for mass production operations, and can meet the needs of mass production, the preparation process cycle is short, and the process Simple process effect

Inactive Publication Date: 2016-11-16
XUCHANG HAOFENG CHEM TECH
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  • Abstract
  • Description
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Problems solved by technology

[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 such an intermediate product; but the traditional preparation process of phenylboronic acid is relatively complicated and not suitable for mass production

Method used

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Embodiment Construction

[0011] In order to make the purpose, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below; it should be understood that the specific implementations described here are only used to explain the present invention, and are not intended to limit the present invention.

[0012] This specific embodiment adopts following technical scheme: its preparation method is:

[0013] Step 1: Under nitrogen protection, add 540g of anhydrous tetrahydrofuran to the reaction flask, start stirring, add 30g of iodobenzene, and cool to -78°C;

[0014] Step 2: Slowly add 86g of n-BuLi (2.0M) dropwise, stir at -78°C for 1.0hr, slowly and naturally rise to 30-40°C to keep warm, and react for 4.0hr;

[0015] Step 3: Cool the reaction solution to below -78°C again, slowly add 77g of triisopropyl borate dropwise, stir for 0.5hr, slowly rise to room temperature, and stir overnight;

[0016] Step 4: Add 540g of 1N hydrochloric a...

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Abstract

The invention discloses a preparation technology of phenylboronic acid reaction liquid, and relates to the technical field of chemical preparation. The preparation technology comprises the following steps of under the protection of nitrogen, enabling anhydrous tetrahydrofuran, iodobenzene and n-BuLi to be subjected to an interaction so as to prepare layered reaction liquid; then through triisopropyl borate, hydrochloric acid and MTBE, obtaining an organic matter; and finally performing extraction and separation on the organic matter so as to obtain phenylboronic acid crude products. The preparation technology is simple in technological process and short in period, mass production requirements can be met, besides, the preparation period is short, and the working efficiency is high.

Description

technical field [0001] The invention relates to the technical field of chemical manufacturing, in particular to a process for preparing a reaction liquid 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 such an intermediate product; but the traditional preparation process of phenylboronic acid is more complicated and not suitable for mass production. Contents of the invention [0003] The object of the present invention is to provide a kind of preparation technology of the reaction solution of phenylboronic acid aiming at the defects and deficiencies of the prior art. [0004] In order to solve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02
CPCC07F5/025
Inventor 骆俊
Owner XUCHANG HAOFENG CHEM TECH
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