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Reacting device used for benzyl brominating of biphenyl derivative and brominating method

A reaction device and derivative technology, applied in the field of biphenyl derivative bromination, can solve the problems of increased difficulty in post-processing, safety risks, low light absorption efficiency, etc., to avoid the use of free radical initiators and facilitate production Scale, the effect of adjusting the production scale

Pending Publication Date: 2019-04-16
LINHAI HUANAN CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because benzyl bromination belongs to the mechanism of free radicals, photoinitiation needs to be used during bromination, and the light absorption efficiency of traditional tank reactors is very low, resulting in the need to add a large amount of free radical initiators such as benzoyl peroxide (BPO ), azobisisobutyronitrile (AIBN), etc. After the reaction, the free radical initiator remains in the waste liquid, which increases the difficulty and safety risk of post-treatment

Method used

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  • Reacting device used for benzyl brominating of biphenyl derivative and brominating method
  • Reacting device used for benzyl brominating of biphenyl derivative and brominating method
  • Reacting device used for benzyl brominating of biphenyl derivative and brominating method

Examples

Experimental program
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Effect test

Embodiment 1

[0118] Dissolve 60g (0.311mol) of 2-cyano-4'methyl biphenyl in 360ml of dichloromethane, stir to dissolve, then weigh 27.84g (0.174mol) of elemental bromine and dissolve it in 2-cyano-4'methyl Stir evenly in the biphenyl solution, as a reaction solution, and store in one of the flasks (the first storage tank); hydrogen peroxide is stored in another flask (the second storage tank); set the first feed pump The flow rate is 22mL / min; the flow rate of the second feed pump is 5mL / min; turn on the LED light and feed pump, control the residence time of the material for 5mins, use water as the temperature control medium, and control the bromination temperature to 25°C-40°C; Collect the reacted materials discharged from the photocatalytic temperature-controlled pipeline reactor with a 500mL four-necked bottle, and quench the remaining elemental bromine and hydrogen peroxide with aqueous sodium sulfite. The layers were separated, the organic layer was spin-dried, and 75.6 g of the produ...

Embodiment 2

[0120] Dissolve 60g (0.125mol) of N-(triphenylmethyl)-5-(4'-methylbiphenyl-2-yl)tetrazolium in 360ml of dichloromethane, stir to dissolve, then weigh the elemental bromine 11g (0.069mol) was dissolved in N-(triphenylmethyl)-5-(4'-methylbiphenyl-2-yl)tetrazolium solution and stirred evenly, as a reaction solution, and stored in one of the flasks (the first storage tank); the hydrogen peroxide is stored in another flask (the second storage tank); the flow rate of the first feed pump is set to 22mL / min; the flow rate of the second feed pump is 5mL / min ;Turn on the LED light and feed pump, control the residence time of the material to 7mins, use water as the temperature control medium, and control the bromination temperature to 25°C-40°C; use a 500mL four-necked bottle to collect After the reaction, the remaining elemental bromine and hydrogen peroxide were quenched with an aqueous solution of sodium sulfite. The layers were separated, the organic layer was spin-dried, and 64.1 g...

Embodiment 3

[0122] Dissolve 60g (0.224mol) of tert-butyl 4'-methyl-[1,1'-biphenyl]-2-carboxylate in 300ml of dichloromethane, stir to dissolve, then weigh 19.7g (0.123mol) of elemental bromine Dissolve in 4'-methyl-[1,1'-biphenyl]-2-formic acid tert-butyl ester solution and stir evenly as a reaction solution, and store in one of the flasks (the first storage tank); hydrogen peroxide Store in another flask (the second storage tank); set the flow rate of the first feed pump to 22mL / min; the flow rate of the second feed pump to 5mL / min; turn on the LED light and feed pump, and the material stays The time is 9mins, water is used as the temperature control medium, and the bromination temperature is controlled at 25°C-40°C; the reacted materials discharged from the photocatalytic temperature-controlled pipeline reactor are collected in a 500mL four-necked bottle, and the remaining Elemental bromine and hydrogen peroxide. Separate the layers, spin dry the organic layer, and recrystallize from a...

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Abstract

The embodiment of the invention provides a reacting device used for benzyl brominating of a biphenyl derivative. The reacting device comprises a first storage tank, a second storage tank, a mixer, a photocatalysis temperature control pipeline reactor and a light source; the first storage tank and the second storage tank are communicated with a feeding port of the mixer; the reactor comprises one or more reaction units; each reaction unit is formed by overlapping three or more transparent flat plates, and a channel is formed between every two adjacent flat plates; each channel comprises one ormore material channels and one or more temperature control channels; the material channels are used for a brominating reaction; the temperature control channels are used for controlling the temperature of the reaction; the light source provides visible light and / or ultraviolet capable of irradiating the material channels. By the adoption of the device and a method, the light absorption rate of thebrominating reaction is high, usage of a free radical initiator is avoided, and the rate of the reaction is also increased; through control over the number and connection mode of the reaction units,the demands of different reaction quantities can be met, and the scale of production is convenient to adjust.

Description

technical field [0001] The invention relates to the technical field of B-position bromination of biphenyl derivatives, in particular to a reaction device for B-position bromination of biphenyl derivatives and a method for applying the same to B-position bromination of biphenyl derivatives. Background technique [0002] Sartan antihypertensive drugs are widely used due to their few adverse reactions, good tolerance, high safety and compliance, and less damage to internal organs such as the heart and kidneys. Among them, losartan, valsartan, and irbesartan have been tested by the market for a long time and are enduring. [0003] [0004] At present, the most important intermediate in the synthesis route of sartan-like APIs is 2-cyano-4'bromomethylbiphenyl, which is the mother nucleus of all sartan-like drugs, and its importance is self-evident. Currently, there are A large number of literatures have reported its synthetic route. [0005] Wherein most of methods are to ado...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/12B01J8/06C07C253/30C07C255/50C07C67/307C07C69/76C07D257/04C07B39/00
CPCB01J8/06B01J19/122C07B39/00C07C67/307C07C253/30C07D257/04C07C255/50C07C69/76
Inventor 张露涂国良何琦杨涛梁尊俊
Owner LINHAI HUANAN CHEM CO LTD
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