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Method for synthesizing 3-methylindole through continuous flow reaction

A technology of methyl indole and reaction, which is applied in the field of synthesizing 3-methyl indole by continuous flow microreactor, can solve the problems of cumbersome purification process, complex reaction process, low yield, etc., and achieve heat and mass transfer efficiency High, high reaction selectivity, fast reaction effect

Active Publication Date: 2017-08-11
QUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the complexity of this type of reaction process, harsh conditions (high temperature for a long time), and many side reactions, the yield is low and the purification process is cumbersome.

Method used

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  • Method for synthesizing 3-methylindole through continuous flow reaction
  • Method for synthesizing 3-methylindole through continuous flow reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Measure 10 mL of ionic liquid 1-ethyl-3-methylimidazolium tetrafluoroboric acid ([emim] BF4) into 50 mL beakers A and B, and measure 20 mL of ionic liquid into 50 mL beaker C middle. Then weigh 1.08g (0.01mol) of phenylhydrazine into beaker A, weigh 0.58g (0.01moL) of propionaldehyde into beaker B, weigh 1.36g (0.01moL) of ZnCl 2 Put the solid into beaker C, stir in the air to make it dissolve evenly.

[0033] (2) Connect the beakers A and B to the metering pumps P1 and P2 respectively, adjust the flow rate (10mL / min), start the pumps P1 and P2 at the same time, and pour the two solutions into the reaction module I.

[0034] (3) The two solutions of A and B are mixed and reacted in the reaction module I at a reaction temperature of 25° C. to generate phenylhydrazone.

[0035] (4) Solution C is connected to pump P3, and after 280s (according to the calculation, it takes 20s for A and B solutions to reach reaction module I, the residence time of reaction solution in...

Embodiment 2

[0040] (1) Measure 10 mL of ionic liquid 1-ethyl-3-methylimidazolium tetrafluoroboric acid ([emim] BF4) into 50 mL beakers A and B, and measure 20 mL of ionic liquid into 50 mL beaker C middle. Then weigh 2.16g (0.02mol) of phenylhydrazine and put it into beaker A, weigh 1.16g (0.02moL) of propionaldehyde and put it into beaker B, and weigh 2.72g (0.02moL) of ZnCl 2 Put the solid into beaker C, stir in the air to make it dissolve evenly.

[0041] (2) Connect the beakers A and B to the metering pumps P1 and P2 respectively, adjust the flow rate (10mL / min), start the pumps P1 and P2 at the same time, and pour the two solutions into the reaction module I.

[0042] (3) The two solutions of A and B are mixed and reacted in the reaction module I at a reaction temperature of 50° C. to generate phenylhydrazone.

[0043] (4) Solution C is connected to pump P3, and after 280s (according to the calculation, it takes 20s for A and B solutions to reach reaction module I, the residence ti...

Embodiment 3

[0048] (1) Measure 10 mL of ionic liquid 1-ethyl-3-methylimidazolium tetrafluoroboric acid ([emim] BF4) into 50 mL beakers A and B, and measure 20 mL of ionic liquid into 50 mL beaker C middle. Then weigh 1.08g (0.01mol) of phenylhydrazine into beaker A, weigh 0.51g (0.01moL) of propionaldehyde into beaker B, weigh 1.36g (0.01moL) of ZnCl 2 Put the solid into beaker C, stir in the air to make it dissolve evenly.

[0049] (2) Connect the beakers A and B to the metering pumps P1 and P2 respectively, adjust the flow rate (10mL / min), start the pumps P1 and P2 at the same time, and pour the two solutions into the reaction module I.

[0050] (3) The two solutions of A and B are mixed and reacted in the reaction module I at a reaction temperature of 75° C. to generate phenylhydrazone.

[0051] (4) Solution C is connected to pump P3, and after 280s (according to the calculation, it takes 20s for A and B solutions to reach reaction module I, the residence time of reaction solution in...

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Abstract

The invention provides a method for synthesizing 3-methylindole through a continuous flow reaction. The synthesis method comprises the steps of mixing and throwing a phenylhydrazine solution and a propionaldehyde solution into a first reaction module separately through a metering pump, wherein the standing time is 3-20 min, and the reaction temperature is 25-75 DEG C; phenylhydrazone is prepared through a reaction, and then when reaction liquid containing phenylhydrazone flows out of the first reaction module, and the metering pump connected with a ZnCl2 solution is started, so that the ZnCl2 solution and the reaction liquid containing phenylhydrazone is mixed and enters a second reaction module which is preheated to 150-200 DEG C, wherein the standing time is 4-10 min, and then reaction liquid which flows out of the second reaction module enters a collection device through a cooling pipe to be preprocessed to obtain the product 3-methylindole. The method for synthesizing 3-methylindole through the continuous flow reaction is high in reaction speed, less in side reaction, high in heat and mass transfer efficiency, high in reaction selectivity, high in purity and high in yield and convenient in aftertreatment, and meanwhile, expensive ionic liquid can be recycled and applied in a re-extraction mode.

Description

[0001] (1) Technical field [0002] The invention relates to a method for preparing 3-methyl indole by a Fisher indole synthesis method, in particular to a method for synthesizing 3-methyl indole by using a continuous flow microreactor. [0003] (2) Background technology [0004] As important N-heterocyclic chemical raw materials, indole compounds are widely used in the synthesis of herbicides, fungicides, dyes and preservatives. And 3-methylindole is also an important medicine and pesticide reagent. It has a strong feces odor, but it has a beautiful floral fragrance after dilution. It is used as a fixative in trace amounts of flower-scented and animal-scented daily essences. , has great application prospect in medicine and fine chemical industry. At present, the traditional kettle-type Fischer indole synthesis technology is adopted in industry. However, due to the complex reaction process, harsh conditions (long time and high temperature), and many side reactions, the yield ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/08
CPCC07D209/08
Inventor 许建帼吕延文余建刚金懿李杰
Owner QUZHOU UNIV
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