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Preparation formula of 4'-bromomethyl-2-cyanobiphenyl

The technology of cyanobiphenyl and bromomethyl is applied in the field of preparation formula of 4'-bromomethyl-2-cyanobiphenyl, and can solve the problems of reducing the bromination reaction speed, slow reaction speed, equipment corrosion and the like, To achieve the effect of easy industrial production, mild reaction conditions, and low equipment corrosiveness

Pending Publication Date: 2020-12-25
安徽太主科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method produces a large amount of by-product hydrogen bromide in the reaction process, and this by-product can suppress the carrying out of bromination reaction, reduces bromination reaction speed, even reacts incompletely, therefore is not suitable for commercial production
[0004] CN101200455A discloses that 4'-methyl-2-cyanobiphenyl reacts with a brominating agent to obtain a product under light conditions, but in a large-scale production process, light energy is difficult to introduce into the reactor interior and bottom, which is not suitable for industrial production
Use HBr / NaBrO3, Br2 / NaBrO3 oxidative bromination system respectively, wherein HBr and Br2 belong to highly corrosive and highly toxic high-risk reagents, corrode equipment, and the operation process is unsafe, and the industrial application value of this method is not high
[0007] WO2011073703 oxidizes the bromination system through NaBrO3 / NaHSO3, the amount of NaBrO3 is three times the amount of the substrate, the amount is large, the cost is high, and it is not suitable for commercial production
[0008] In summary, the preparation of 4'-bromomethyl-2-cyanobiphenyl has slow reaction speed, low industrial application value, high production cost, corrosion to equipment, unsafe operation, high cost, and is not suitable for industrial production

Method used

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  • Preparation formula of 4'-bromomethyl-2-cyanobiphenyl

Examples

Experimental program
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Embodiment 1

[0031] A preparation formula of 4'-bromomethyl-2-cyanobiphenyl according to the present invention is made of the following raw materials in parts by weight: 550-650 parts of organic solvent, 550-650 parts of water, 4'-methanol 190-195 parts of base-2-cyanobiphenyl, 60-85 parts of bromide salt, 45-55 parts of bromate or chlorate, 150-250 parts of hydrochloric acid solution, and 450-550 parts of recrystallization solvent.

[0032] Further, the concentration of the hydrochloric acid is 15-30%.

[0033] Further, the recrystallization solvent is toluene or ethyl acetate or tert-butyl methyl ether or water.

[0034] Further, the recrystallization solvent is toluene.

[0035] Further, the bromide salt is sodium bromide or potassium bromide or lithium bromide or magnesium bromide or calcium bromide.

[0036] Further, the bromide salt is sodium bromide or potassium bromide.

[0037] Further, the bromate is sodium bromate or potassium bromate or lithium bromate or magnesium bromate o...

Embodiment 2

[0042] A preparation formula of 4'-bromomethyl-2-cyanobiphenyl according to the present invention is made of the following raw materials in parts by weight: 600 parts of organic solvent, 600 parts of water, 4'-methyl-2- 103 parts of cyanobiphenyl, 69 parts of bromide salt, 50 parts of bromate or chlorate, 200 parts of hydrochloric acid solution, and 500 parts of recrystallization solvent.

[0043] Further, the concentration of the hydrochloric acid is 15-30%.

[0044] Further, the recrystallization solvent is toluene or ethyl acetate or tert-butyl methyl ether or water.

[0045] Further, the recrystallization solvent is toluene.

[0046] Further, the bromide salt is sodium bromide or potassium bromide or lithium bromide or magnesium bromide or calcium bromide.

[0047] Further, the bromide salt is sodium bromide or potassium bromide.

[0048] Further, the bromate is sodium bromate or potassium bromate or lithium bromate or magnesium bromate or calcium bromate or sodium chlo...

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Abstract

The invention relates to the technical field of pharmaceutical chemicals, and particularly discloses a preparation formula of 4'-bromomethyl-2-cyanobiphenyl. The 4'-bromomethyl-2-cyanobiphenyl is prepared from, by weight, 550-650 parts of an organic solvent, 550-650 parts of water, 190-195 parts of 4'-methyl-2-cyanobiphenyl, 60-85 parts of bromide, 45-55 parts of bromate or chlorate, 150-250 partsof a hydrochloric acid solution and 450-550 parts of a recrystallization solvent. The formula overcomes the defects of the prior art, and has the advantages of mild reaction conditions, high reactionselectivity, fewer byproducts, low equipment corrosion, simple operation, low cost, low environmental protection pressure, easy product separation, safe and easy operation of bromination reagents, high bromine atom utilization rate, easy industrial production and high product purity.

Description

technical field [0001] The invention relates to the technical field of medicine and chemical industry, in particular to a preparation formula of 4'-bromomethyl-2-cyanobiphenyl. Background technique [0002] Sartan drugs are the first-line antihypertensive drugs, which have a brand-new antihypertensive mechanism, stable antihypertensive effect, good curative effect, long duration of action, and good patient tolerance. Most of the sartan drugs need to be prepared through the intermediate 4'-bromomethyl-2-cyanobiphenyl. The currently disclosed synthetic methods are as follows: [0003] US5621134 describes the preparation of 4'-bromomethyl-2-cyanobiphenyl from inexpensive bromine in the presence of free radical initiating reagents. But this method produces a large amount of by-product hydrogen bromide in the reaction process, and this by-product can suppress the carrying out of bromination reaction, reduces bromination reaction speed, even reaction is incomplete, therefore is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C253/34C07C255/50
CPCC07C253/30C07C253/34C07C255/50
Inventor 欧阳细妹
Owner 安徽太主科技发展有限公司
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