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Method for preparing fluorinating reagent and fluoride continuously by microchannel reactor

A technology of microchannel reactors and fluorinated reagents, applied in the preparation of amino compounds by condensation/addition reactions, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of fluorinated reagents and fluorides, energy consumption and Problems such as high environmental protection cost and low production efficiency achieve the effect of low production cost, shortened production cycle and improved production efficiency

Inactive Publication Date: 2019-05-21
JIANGSU HANSYN PHARMA
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Problems solved by technology

[0006] In view of the fact that the current preparation methods of fluorinated reagents and fluorides mainly adopt the kettle reaction method, the production efficiency is low, the cycle is long, the solvent consumption is large, and the energy consumption and environmental protection costs are high.
So far, there has been no report on the process of producing and preparing fluorinated reagents and fluorides in a microchannel continuous flow mode. preparation of

Method used

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  • Method for preparing fluorinating reagent and fluoride continuously by microchannel reactor
  • Method for preparing fluorinating reagent and fluoride continuously by microchannel reactor
  • Method for preparing fluorinating reagent and fluoride continuously by microchannel reactor

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Experimental program
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Effect test

Embodiment 1

[0043] The preparation of embodiment 1 Ishikawa reagent

[0044] The device used: high-throughput microchannel reactor, refer to Figure 4 Microchannel reactor continuous flow synthesis process flow diagram.

[0045] The diethylamine solution that needs to enter the microchannel reactor is prepared in advance, the flow rate ratio of the relevant materials is preset through the flow meter, the speed of the feed pump is adjusted, and the ratio of the materials is kept within a certain range. Among them, diethylamine: The mass ratio of dichloromethane is 1:1, that is, 200g diethylamine (2.74mol, 1.0eq) and 200g dichloromethane are formulated into a solution, and diethylamine solution and 411g hexafluoropropylene (2.74mol, 1.0eq) are respectively It is introduced into functional module a through a feeding pump, the reaction temperature is set at 20°C, and the reaction residence time is 90 seconds. The collected liquid flowing out of functional module A is the Ishikawa reagent, an...

Embodiment 2

[0046] The preparation of embodiment 2 Yarowenko reagent

[0047] The device used: high-throughput microchannel reactor, refer to Figure 4 Microchannel reactor continuous flow synthesis process flow diagram.

[0048] The diethylamine solution that needs to enter the microchannel reactor is prepared in advance, and the flow rate ratio of relevant materials is preset by a flowmeter, wherein diethylamine: the mass ratio of dichloromethane is 1:0.8, that is, 200g diethylamine ( 2.74mol, 1.0eq) and 160g of dichloromethane are prepared into a solution, and the diethylamine solution and 319g of chlorotrifluoroethylene (2.74mol, 1.0eq) are respectively introduced into functional module a through a feed pump, and the reaction temperature is set at 20°C , the reaction residence time is 90 seconds, and the liquid flowing out from the functional module a is collected as the Yarowenko reagent, and the reaction is a quantitative reaction.

Embodiment 3

[0049] The preparation of embodiment 3 TFEDMA reagent

[0050] The device used: high-throughput microchannel reactor, refer to Figure 4 Microchannel reactor continuous flow synthesis process flow diagram.

[0051] The diethylamine solution that needs to enter the microchannel reactor is prepared in advance, and the flow rate ratio of the relevant materials is preset by the flow meter, wherein diethylamine: the mass ratio of dichloromethane is 1:0.9, that is, 200g diethylamine ( 2.74mol, 1.0eq) and 180g of dichloromethane are prepared into a solution, and the diethylamine solution and 274g of tetrafluoroethylene (2.74mol, 1.0eq) are respectively introduced into the functional module a through the feeding pump, and the reaction temperature is set at 20°C. The reaction residence time is 95 seconds, and the liquid flowing out from the functional module a is collected as the Yarowenko reagent, and the reaction is a quantitative reaction.

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Abstract

The invention discloses a method for preparing a fluorinating reagent and fluoride continuously by a microchannel reactor. The method comprises the following steps: introducing a mixed solution of amine and a solvent as well as fluorine-containing olefin into the microchannel reactor separately, performing reaction at the reaction temperature of subzero 20 to 30 DEG C for 30 to 180 seconds to prepare the fluorinating reagent, introducing the fluorinating reagent and a compound A into the microchannel reactor, performing mixing, heating and reaction to obtain a compound B, and performing hydrolysis reaction on the reaction liquid of the compound B to obtain a compound C. The method is simple to operate and safe to use, the use amount of the materials is greatly reduced, the process is environmentally-friendly and continuous, and the risk of high pressure and high temperature is avoided, so that high-yield continuous production of the fluorinating agent or fluoride is feasible. The comprehensive yield of the fluoride reaches 90 to 95 percent, basic quantitative reaction of the fluorinating reagent is realized and industrialized production is facilitated.

Description

technical field [0001] The invention relates to a new method for continuously preparing fluorinated reagents and fluorides by using a microchannel reactor, which belongs to the technical field of organic synthesis applications. Background technique [0002] Fluorinated reagents (Ishikana's Reagent or Yarovenko Reagent or TFEDMA) are widely used in the development of pesticides, veterinary drugs, human drugs and some fine chemicals. Fluorides often have more special physical and chemical properties than conventional substances, especially in pharmaceutical research On the surface, fluoride occupies a considerable part of the proportion. In the fluorination reaction, the hydroxyl group in the compound is reacted by a fluorinating reagent, and the hydroxyl group is replaced by fluorine. This is a large class of reactions that introduce fluorine in the current drug synthesis method, and it has been widely used in the synthesis of many fluorine-containing drugs. application. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/40C07C315/04C07C209/60C07C211/15C07D263/14B01J19/00
Inventor 王希林丁尊良胡振宇
Owner JIANGSU HANSYN PHARMA
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