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Method for continuously preparing 2-aryl-benzothiophene/furan compound by utilizing electrochemical micro-channel reaction device

A technology of microchannel reaction and benzothiophene, applied in the direction of electrodes, electrolysis process, electrolysis components, etc., can solve the problems of high reactor design requirements, poor selectivity, environmental pollution, etc., and achieve good industrial application prospects and reaction temperature Low, high safety effect

Active Publication Date: 2020-02-14
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved in the present invention is to provide a method for continuously preparing 2-aryl-benzothiophene / furan compounds using an electrochemical microchannel reaction device, so as to solve the environmental pollution problem and the impact on the reactor in the prior art. High design requirements, poor selectivity, high energy consumption, etc.

Method used

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  • Method for continuously preparing 2-aryl-benzothiophene/furan compound by utilizing electrochemical micro-channel reaction device
  • Method for continuously preparing 2-aryl-benzothiophene/furan compound by utilizing electrochemical micro-channel reaction device
  • Method for continuously preparing 2-aryl-benzothiophene/furan compound by utilizing electrochemical micro-channel reaction device

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Experimental program
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Effect test

Embodiment 1

[0035] Assemble the electrochemical flow cell device: select the carbon sheet as the anode electrode, place it on the lower layer of the titanium alloy electrolytic cell bracket, and then place the PTFE reaction tank with a volume of 0.5ml on the upper layer of the carbon sheet, and then plate the cathode with platinum The titanium alloy plate is placed on the upper layer of the reaction tank, and finally fixed with a polytetrafluoroethylene screw and connected to an adjustable DC power supply. Weigh 0.045g of 2-phenylethynylanisole sulfide and 0.0332g of KI and dissolve them in 1ml of water and 5ml of acetonitrile to prepare a homogeneous solution A. The prepared homogeneous solution A was passed into the reaction module with a single-stream injection at a flow rate of 0.02 ml / min using a syringe pump. Turn on the power supply, adjust the current to 20mA, and collect the product 2-phenyl-benzothiophene from the outlet of the reaction module after it stabilizes.

[0036] NMR ...

Embodiment 2

[0038]Assemble the electrochemical flow cell device: select the carbon sheet as the anode electrode, place it on the lower layer of the titanium alloy electrolytic cell bracket, and then place the PTFE reaction tank with a volume of 0.5ml on the upper layer of the carbon sheet, and then plate the cathode with platinum The titanium alloy plate is placed on the upper layer of the reaction tank, and finally fixed with a polytetrafluoroethylene screw and connected to an adjustable DC power supply. Weigh 0.045g of 2-phenylethynylanisole sulfide and 0.03g of NaI and dissolve them in 1ml of water and 5ml of acetonitrile to prepare a homogeneous solution A. The prepared homogeneous solution A was passed into the reaction module with a single-stream injection at a flow rate of 0.02 ml / min using a syringe pump. Turn on the power supply, adjust the current to 20mA, and collect the product 2-phenyl-benzothiophene from the outlet of the reaction module after it stabilizes.

Embodiment 3

[0040] Assemble the electrochemical flow cell device: select the carbon sheet as the anode electrode, place it on the lower layer of the titanium alloy electrolytic cell bracket, and then place the PTFE reaction tank with a volume of 0.5ml on the upper layer of the carbon sheet, and then plate the cathode with platinum The titanium alloy plate is placed on the upper layer of the reaction tank, and finally fixed with a polytetrafluoroethylene screw and connected to an adjustable DC power supply. Weigh 0.045g of 2-phenylethynylanisole sulfide and 0.074g of Bu 4 NI was dissolved in 1 ml of water and 5 ml of acetonitrile to make a homogeneous solution A. The prepared homogeneous solution A was passed into the reaction module with a single-stream injection at a flow rate of 0.02 ml / min using a syringe pump. Turn on the power supply, adjust the current to 20mA, and collect the product 2-phenyl-benzothiophene from the outlet of the reaction module after it stabilizes.

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Abstract

The invention discloses a method for continuously preparing a 2-aryl-benzothiophene / furan compound by utilizing an electrochemical micro-channel reaction device. The preparation method comprises the following steps: dissolving ethynyl thioanisole / phenylethynyl anisole and an iodine-containing electrolyte in water and acetonitrile to prepare a homogeneous solution, then introducing the prepared homogeneous solution into a feeding hole of an electrochemical micro-channel reaction device by utilizing an injection pump in single-strand sample introduction, and reacting under the action of a direct-current power supply to obtain the product 2-aryl-benzothiophene / furan compound; wherein the electrochemical micro-channel reaction device comprises an anode electrode, a cathode electrode, an electrolytic tank bracket, a reaction tank, the direct-current power supply and a temperature control module; wherein the reaction tank is positioned between the anode electrode and the cathode electrode, and a closed serpentine flow path is formed between the anode electrode and the cathode electrode; the anode electrode and the cathode electrode are arranged on the electrolytic tank bracket; one endsof the anode electrode and the cathode electrode are connected with each other and are connected with the direct-current power supply; and the temperature control module is embedded in the electrolytic tank bracket and is used for controlling the temperature of liquid in the reaction tank.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for continuously preparing 2-aryl-benzothiophene / furan compounds by using an electrochemical microchannel reaction device. Background technique [0002] 2-Phenyl-benzothiophene and its derivatives are sulfur-containing heterocyclic compounds that widely exist in nature. They are important intermediates in organic synthesis and are widely used in the synthesis of functional materials such as medicine, pesticides and semiconductors. , and its synthesis has attracted widespread attention. At present, there are three main routes for the preparation of 2-aryl-benzothiophenes: (1) 2-arylation reaction of benzothiophene; (2) reaction of 2-boronic acid benzothiophene with aryl donor Coupling reaction; (3) prepared by intramolecular cyclization of substituted benzene derivatives. [0003] 2-Aryl-benzofuran compounds and their derivatives widely exist in natural and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/02C25B9/06C25B11/04C25B3/23C25B9/17
CPCC25B11/04C25B3/23C25B9/17
Inventor 郭凯张东方正蔡谨琳刘成扣朱宁张锴欧阳平凯
Owner NANJING UNIV OF TECH
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