Continuous flow method for synthesizing p-bromo-methyl biphenyl carbonitrile and reaction device thereof

A technology of bromomethylbiphenylcyanonitrile and methylbiphenylcyanonitrile, which is applied in the field of continuous flow and reaction devices for synthesizing p-bromomethylbiphenylcyanonitrile, can solve the problem of low utilization rate of bromine atoms and the like , to achieve the effect of strong industrial application value, good safety and improved utilization rate

Pending Publication Date: 2020-11-20
ZHEJIANG KINGLYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0020] In summary, the first two methods in the above-mentioned methods have the problem of recycling bromine atom carrier molecules, while the latter two methods have the disadvantage of low utilization rate of bromine atoms

Method used

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  • Continuous flow method for synthesizing p-bromo-methyl biphenyl carbonitrile and reaction device thereof
  • Continuous flow method for synthesizing p-bromo-methyl biphenyl carbonitrile and reaction device thereof
  • Continuous flow method for synthesizing p-bromo-methyl biphenyl carbonitrile and reaction device thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Reactor such as figure 1 shown. The length of the reactor pipe is 40m, the diameter is 3mm, the pipe material is Teflon, and the light source is a 405nm purple LED lamp.

[0058] First open the semiconductor temperature control box 10 precooling pipelines, the temperature is set at 12 ℃, add 15% aqueous sodium carbonate solution in the quenching agent aqueous solution liquid storage tank 15; 19.3 grams (0.1mol) p-methylbiphenylcarbonitrile is dissolved in Store 200mL of dichloromethane in p-methylbiphenylcyanonitrile liquid storage tank 1, add a sufficient amount of 40% hydrobromic acid in hydrobromic acid aqueous solution liquid storage tank 2, add sufficient amount of hydrogen peroxide aqueous solution liquid storage tank 3 30% hydrogen peroxide; after opening the built-in LED light source 14, start each pump to pump the material, adjust each pump speed to make p-methylbiphenylcyanonitrile: hydrobromic acid: hydrogen peroxide mol ratio is controlled at 1:1.1:1.2, con...

Embodiment 2

[0060] Reactor such as figure 1 shown. The length of the reactor pipe is 40m, the diameter is 3mm, the pipe material is Teflon, and the light source is a 475nm blue LED lamp.

[0061] First open the semiconductor temperature control box 10 precooling pipelines, the temperature is set at 13 ° C, add 15% aqueous sodium bicarbonate solution in the quenching agent aqueous solution liquid storage tank 15; 19.3 grams (0.1mol) p-methylbiphenylcarbonitrile is dissolved Store in 200mL ethyl acetate in p-methylbiphenyl cyanonitrile liquid storage tank 1, add sufficient amount of 40% hydrobromic acid in hydrobromic acid aqueous solution liquid storage tank 2, add sufficient amount of 30% hydrobromic acid in liquid storage tank 3 % hydrogen peroxide; After opening the built-in LED light source 14, start each pump to pump the material, adjust each pump speed to make p-methylbiphenylcyanonitrile: hydrobromic acid: hydrogen peroxide mol ratio is controlled at 1:1.2:1.4, control the reaction...

Embodiment 3

[0063] The structure of the reaction device is as figure 1 As shown, the length of the reactor pipe is 45m, the diameter is 3mm, the pipe material is Teflon, and the light source is a 565nm yellow-green LED lamp.

[0064] First open the semiconductor temperature control box 10 pre-cooling pipelines, the temperature is set at 14 ℃, add 15% aqueous sodium carbonate solution in the quenching agent aqueous solution liquid storage tank 15; 19.3 grams (0.1mol) p-methylbiphenylcarbonitrile is dissolved in 200mL of ethyl acetate is stored in the p-methylbiphenylcyanonitrile storage tank 1, a sufficient amount of 40% hydrobromic acid is added to the hydrobromic acid aqueous solution storage tank 2, and a sufficient amount of 40% hydrobromic acid is added to the hydrogen peroxide aqueous solution storage tank 3 30% hydrogen peroxide; Open the built-in LED light source 14, start each pump to pump the material, adjust each pump speed to make p-methylbiphenylcyanonitrile: hydrobromic acid:...

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Abstract

The invention discloses a continuous flow method for synthesizing p-bromo-methyl biphenyl carbonitrile and a reaction device for synthesizing p-bromo-methyl biphenyl carbonitrile. P-methyl biphenyl carbonitrile is used as a raw material; bromine generated by oxidizing hydrobromic acid through hydrogen peroxide is used as a bromination reagent; materials are continuously input into an efficient mixer through a metering pump to be mixed and then enter a pipeline reactor; and temperature control and illumination on reactants in the pipeline reactor are carried out to complete bromination reaction, quenching of a reaction liquid in the pipeline reactor is carried out, continuous liquid separation, and drying, concentration and recrystallization purification on the obtained organic phase are carried out to obtain the pure p-bromo-methyl biphenyl carbonitrile product. The bromination reaction has the advantages of high bromine atom utilization rate, fewer byproducts and fewer solid wastes, and conforms to the concept of green chemistry; the continuous flow synthesis method has the advantages of good safety, convenience in intelligent control, short reaction time, high post-treatment efficiency and the like, and has industrial production and application values.

Description

technical field [0001] The invention discloses a continuous flow method and a reaction device for synthesizing p-bromomethylbiphenylcyanonitrile. Background technique [0002] Sartan-like antihypertensives are a new class of antihypertensive drugs widely used in clinical practice. This type of antihypertensive drug has the advantages of obvious antihypertensive effect, good tolerance, and small side effects, and also has a certain therapeutic effect on heart failure, myocardial infarction, diabetes and other cardiovascular and cerebrovascular diseases. It has been recommended by multiple treatment guidelines of the International Health Organization as the first-line antihypertensive drug for hypertensive patients with cardiovascular disease and proteinuria. [0003] Continuous flow chemical reaction (Flow Chemical Reaction) is to pump two or more different gaseous, liquid or semi-solid reactants to a microchannel reactor, tubular reactor or small tank reactor at a given flo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/50C07C253/30C07C253/34
CPCC07C253/30C07C253/34C07C255/50
Inventor 张晓伟赵斌锋严成松金红卫章治国刘道宏
Owner ZHEJIANG KINGLYUAN PHARMA
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