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Preparation method of 4'-bromomethyl-2-cyanobiphenyl dissolved in 1,2-dichloroethane

A technology of bromosartan biphenyl and dichloroethane, which is applied in the field of medicine and chemical industry, can solve the problems of uneven distribution of reactants, increased waste water treatment pressure, high raw material cost, etc., achieves excellent atom economy, and reduces treatment costs Difficulty and the effect of reducing security risks

Inactive Publication Date: 2020-06-26
JIAXING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But above-mentioned preparation method utilizes N-hydroxyphthalimide etc. as free radical initiator, and excessive raw material cost is unfavorable for industrial popularization, especially the use of water seal has increased the pressure of wastewater treatment after reaction, unsuitable in actual production
[0006] In particular, the above-mentioned method has a long preparation period and a large proportion of feeding materials, which cannot be applied to the technological change trend of continuous and semi-continuous automatic production lines in actual industrial production.
Moreover, the existing tank reaction has the problems of uneven distribution of reactants, high risk of potential local overheating, and time-consuming problems of loading and unloading
[0007] Therefore, the development of a method for preparing 2-cyano-4'-bromomethylbiphenyl with high atomic conversion rate and low safety risk, which can be applied to automated continuous production lines has become an urgent problem for those skilled in the art.

Method used

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  • Preparation method of 4'-bromomethyl-2-cyanobiphenyl dissolved in 1,2-dichloroethane
  • Preparation method of 4'-bromomethyl-2-cyanobiphenyl dissolved in 1,2-dichloroethane
  • Preparation method of 4'-bromomethyl-2-cyanobiphenyl dissolved in 1,2-dichloroethane

Examples

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Effect test

Embodiment 1

[0037]A method for preparing bromosartan biphenyl dissolved in 1,2-dichloroethane, dissolving 10g of 2-cyano-4-methyl biphenyl in 30mL of 1,2-dichloroethane, and loading it into a syringe In tube A; dissolve 9 g of N-bromosuccinimide in 30 mL of 1,2-dichloroethane and put it into tube B of the syringe. Install the two syringes A and B on the flow syringe pump, and set the flow rates of the two tubes A and B to be 1.5 mL / min. Turn on the constant temperature water bath device, heat to 70°C, keep the temperature, turn on the 4000K LED light at 365nm for 30min, and turn on the flow reactor at the same time. After the reaction is completed, add 15 g of sodium bisulfite to the received product to quench, separate the liquid, remove the solvent by rotary evaporation of the organic phase, add isopropyl ether for recrystallization, suction filtration, and put the filter cake in an oven to dry to obtain a pure product. The product, 2-cyano-4'-bromomethylbiphenyl, has a purity of 93% a...

Embodiment 2

[0039] A method for preparing bromosartan biphenyl dissolved in 1,2-dichloroethane, dissolving 11g of 2-cyano-4-methylbiphenyl in 30mL of 1,2-dichloroethane and filling it into a syringe In tube A; dissolve 7 mL of bromine in 30 mL of 1,2-dichloroethane and put it into tube B of the syringe. Install the two syringes A and B on the flow syringe pump, and set the flow rates of the two tubes A and B to be 1.5 mL / min. Turn on the constant temperature water bath device, heat to 70°C, keep the temperature, turn on the 4000K LED light at 365nm for 30min, and turn on the flow reactor at the same time. After the reaction is completed, add 15 g of sodium bisulfite to the received product to quench, separate the liquid, remove the solvent by rotary evaporation of the organic phase, add isopropyl ether for recrystallization, suction filtration, and put the filter cake in an oven to dry to obtain a pure product. The product, 2-cyano-4'-bromomethylbiphenyl, has a purity of 92% and a yield ...

Embodiment 3

[0041] A method for preparing bromosartan biphenyl dissolved in 1,2-dichloroethane, dissolving 11g of 2-cyano-4-methylbiphenyl in 30mL of 1,2-dichloroethane and filling it into a syringe In tube A; dissolve 4 g of sodium bromide and 3 g of sodium bromate in 30 mL of 1,2-dichloroethane, and put them into tube B of the syringe. Install the two syringes A and B on the flow syringe pump, and set the flow rates of the two tubes A and B to be 1.5 mL / min. Turn on the constant temperature water bath device, heat to 70°C, keep the temperature, turn on the 4000K LED light at 365nm for 30min, and turn on the flow reactor at the same time. After the reaction is completed, add 15 g of sodium bisulfite to the received product to quench, separate the liquid, remove the solvent by rotary evaporation of the organic phase, add isopropyl ether for recrystallization, suction filtration, and put the filter cake in an oven to dry to obtain a pure product. The product, 2-cyano-4'-bromomethylbipheny...

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Abstract

The invention discloses a preparation method of 4'-bromomethyl-2-cyanobiphenyl dissolved in 1,2-dichloroethane, belongs to the technical field of pharmaceutical chemicals, and particularly discloses amethod for preparing substituent-containing 4'-bromomethyl-2-cyanobiphenyl by using a flowing photochemical method. Methyl biphenyl is used as a raw material, 1,2-dichloroethane is used as a solvent,a composition of a bromination reagent, dibromohydantoin, N-bromosuccinimide or sodium bromide and sodium bromate is used as a bromination reagent, and after the raw materials and the bromination reagent are mixed with the solvent, the obtained mixtures flow into a pipeline through injection pipes, and are mixed through a mixer, and the obtained mixture enters a constant-temperature water bath reactor and is subjected to a reaction through illumination. The 4'-bromomethyl-2-cyanobiphenyl synthesized by the preparation method is good in purity, high in yield, simple in reaction system, low intoxicity and high in atom conversion rate, is suitable for industrial application in the field of biological medicines, can be suitable for an automatic continuous production process, and conforms tothe development concepts of green chemical industry, high efficiency and economy.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a preparation method of bromosartan biphenyl dissolved in 1,2-dichloroethane. Background technique [0002] Sartans are the first-line antihypertensive drugs, with a new antihypertensive mechanism, stable blood pressure, good curative effect, long duration of action, and good patient tolerance. Angiotensin II receptor antagonist (ARB) class of antihypertensive drugs ("sartan" drugs) has been in existence for more than 20 years, because of its obvious antihypertensive effect and good tolerance, especially clinical trial data show that it has anti-cardiac effects. The unique curative effect and protective effect of vascular disease have become one of the most common antihypertensive drugs in clinical practice. The incidence of adverse reactions such as dry cough, rebound after drug withdrawal, orthostatic hypotension, elevated serum potassium and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/50
CPCC07C253/30C07C255/50
Inventor 张俊勇徐昊潘伟谢景力
Owner JIAXING UNIV
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