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Method for tubular reaction preparation of substituted benzylically brominated methyl biphenyl and reaction device of method

A technology of methyl biphenyl and reaction device, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid nitrile, etc., can solve problems such as difficult separation and extraction, long reaction time, low conversion rate, etc., and achieve reaction control Simple, convenient after-treatment, and less by-product formation

Inactive Publication Date: 2018-04-20
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In summary, the common problems of the above traditional synthesis methods are: long reaction time, low conversion rate, many by-products, difficult separation and extraction, and potential environmental safety hazards

Method used

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  • Method for tubular reaction preparation of substituted benzylically brominated methyl biphenyl and reaction device of method
  • Method for tubular reaction preparation of substituted benzylically brominated methyl biphenyl and reaction device of method
  • Method for tubular reaction preparation of substituted benzylically brominated methyl biphenyl and reaction device of method

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Experimental program
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Embodiment 1

[0035] The structure of the special reaction device used in this embodiment is as follows: figure 1 As shown, the reactor 8 adopts a pipeline with a length of 30m and a diameter of 2mm, and the material of the pipeline is a polytetrafluoroethylene tube; the light source 6 is a UV lamp with a wavelength of 250nm.

[0036] First turn on the light source 6, turn on the internal circulation constant temperature water bath 7 to preheat the pipeline, add 100mL of water to the receiving tank 10, and set the reaction temperature to 77°C; Tetrazolium]-4-methylbiphenyl and 12.8 g (0.08 mol) of bromine were dissolved in 480 mL of ethyl acetate and stored in the storage tank a1; 17.5 g of 30% hydrogen peroxide (0.15 mol) was added to the storage solution In the tank b2, turn on the infusion pump a4 and the infusion pump b5, adjust the flow rate, and continuously input 2'-[(N-trityl)tetrazolium]-4-methylbiphenyl, bromine and hydrogen peroxide into the tank b2 respectively Mix in the high-...

Embodiment 2

[0038] The structure of the reaction device is as figure 1 , the reactor 8 adopts a pipeline with a length of 50m and a diameter of 2mm, and the material of the pipeline is a polytetrafluoroethylene tube; the light source 6 is a UV lamp with a wavelength of 250nm.

[0039] First turn on the light source 6, turn on the internal circulation constant temperature water bath 7 to preheat the pipeline, add 100mL of water to the receiving tank 10, and the reaction temperature is 78°C; Azole]-4-methylbiphenyl and 32.0g (0.2mol) bromine were dissolved in 240mL ethyl acetate and stored in the liquid storage tank a1 and liquid storage tank b2 respectively, and the infusion pump a4 and the infusion pump b5 were turned on , adjust the flow rate, continuously input 2′-[(N-trityl)tetrazolium]-4-methylbiphenyl and bromine into the high-efficiency mixer 3 for mixing, and then enter the internal circulation constant temperature water bath React in the pipeline of 7 inner light, reaction time 1...

Embodiment 3

[0041] The structure of the reaction device is as figure 1 , the reactor 8 adopts a pipeline with a length of 100 m and a diameter of 2 mm, and the material of the pipeline is a polytetrafluoroethylene tube; the light source 6 is a 250nm UV lamp.

[0042] First turn on the light source 6, turn on the internal circulation constant temperature water bath 7 to preheat the pipeline, add 100mL water to the receiving tank 10, and the reaction temperature is 78°C; Azole]-4-methylbiphenyl and 32.0g (0.2mol) bromine were respectively dissolved in 240mL ethyl acetate and stored in liquid storage tank a1 and liquid storage tank b2 respectively, and the infusion pump a4 and infusion pump b5 were turned on, Adjust the flow rate, respectively input 2'-[(N-trityl)tetrazolium]-4-methylbiphenyl and bromine continuously into the high-efficiency mixer 3 for mixing, and then enter the inner circulation constant temperature water bath 7 Carry out the reaction in the pipeline of internal light, th...

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Abstract

The invention discloses a method for tubular reaction preparation of substituted benzylically brominated methyl biphenyl and a reaction device of the method. According to the method, substituted methyl biphenyl is taken as a raw material and bromine is taken as a bromination reagent. The reaction materials are continuously fed into a high-efficiency mixer for mixing through a liquid conveying pump, and the formed mixture enters a reactor in a water bath for a reaction, after the reaction is finished, the reaction system enters a receiving tank, a reducing agent is added to the receiving tank for quenching, liquid separation is carried out, anhydrous sodium sulfate is added into the organic phase, suction filtration is performed, the organic phase is subjected to reduced-pressure concentration for solvent removal, a solvent is added for recrystallization, suction filtration is performed, and the filter cake is dried to obtain a pure product namely the substituted benzylically brominatedmethyl biphenyl. The method of the invention is simple and convenient to control, high in safety, less in generation of by-products and convenient for post-processing, a small trial process can be directly used for amplified production. The method meets the requirements of green chemistry and has a certain industrial application value.

Description

technical field [0001] The invention discloses a method and a special device for pipelined benzyl bromination, in particular to a pipelined method for preparing benzyl bromomethylbiphenyl containing substituents and a reaction device thereof. The compound is sartan Important intermediates of antihypertensive drugs. Background technique [0002] Angiotensin II receptor antagonist (ARB) antihypertensive drugs ("sartan" drugs) have been available for more than 20 years, because of their obvious antihypertensive effect and good tolerance, especially the clinical trial data show that they have antihypertensive effect on the heart. The unique curative effect and protective effect on vascular diseases have become one of the most common antihypertensive drugs in clinical practice. The incidence of adverse reactions such as dry cough, drug withdrawal rebound, orthostatic hypotension, elevated blood potassium and serum creatinine after long-term use of the drug is low, and it has bee...

Claims

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Application Information

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IPC IPC(8): C07D257/04C07C253/30C07C255/50
CPCC07D257/04C07C253/30C07C255/50
Inventor 李坚军李传兵孙坚裴金凤苏为科
Owner ZHEJIANG UNIV OF TECH
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