Continuous synthesis method of 2, 3-dimethylphenylsulfide

A technology of dimethyl anisole and synthetic method, which is applied to the preparation of sulfide, chemical instruments and methods, and the preparation of organic compounds, etc., which can solve the problems of low efficiency of mass transfer and heat transfer, long production cycle, cumbersome operation steps, etc. problems, achieve the effect of safe and stable synthesis method, reduce production cost, and simplify the operation process

Pending Publication Date: 2022-04-12
山东亿盛实业股份有限公司
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Problems solved by technology

[0005] Aiming at the problems of low mass and heat transfer efficiency, long production cycle, cumbersome operation steps, poor safety performance and low equipment utilization rate in the preparation of 2,3-dimethylanisole in the prior art, the present invention Provide a kind of continuous synthetic method of 2,3-dimethyl anisole, to solve the above problems

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  • Continuous synthesis method of 2, 3-dimethylphenylsulfide
  • Continuous synthesis method of 2, 3-dimethylphenylsulfide
  • Continuous synthesis method of 2, 3-dimethylphenylsulfide

Examples

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Embodiment 1

[0023] A method for preparing 2,3-dimethylanisole, the specific steps are as follows:

[0024] Microchannel reactor model: RMCS1010, with a total of ten reaction modules, of which the 1st to 5th reaction modules are the first reaction area, the 6th to 10th reaction modules are the second reaction area, A channel and B channel are connected with the first The reaction modules are connected, and the C channel is connected to the sixth reaction module; the liquid holding capacity of each reaction module is 0.75mL, and the liquid holding capacity of the pipeline and joint is 2.9mL; the infusion pump model: PF100 semi-preparative medium-pressure infusion pump.

[0025] (1) controlling the temperature of the first reaction zone and the second reaction zone to be 0°C;

[0026] (2) Place 700 g of hydrochloric acid solution with 100 g of 2,3-dimethylaniline in the storage bottle of channel A; place 180 g of aqueous solution of 70 g of sodium nitrite in the storage bottle of channel B; ...

Embodiment 2

[0032] A method for preparing 2,3-dimethylanisole, the specific steps are as follows:

[0033] Microchannel reactor model: RMCS1010, with a total of ten reaction modules, of which the 1st to 5th reaction modules are the first reaction area, the 6th to 10th reaction modules are the second reaction area, A channel and B channel are connected with the first The reaction modules are connected, and the C channel is connected to the sixth reaction module; the liquid holding capacity of each reaction module is 0.75mL, and the liquid holding capacity of the pipeline and joint is 2.9mL; the infusion pump model: PF100 semi-preparative medium-pressure infusion pump.

[0034] (1) Control the temperature of the first reaction zone and the second reaction zone to be 5°C;

[0035] (2) Place 690 g of hydrochloric acid solution with 100 g of 2,3-dimethylaniline in the storage bottle of channel A; place 180 g of aqueous solution of 70 g of sodium nitrite in the storage bottle of channel B; The...

Embodiment 3

[0041] A method for preparing 2,3-dimethylanisole, the specific steps are as follows:

[0042] Microchannel reactor model: RMCS1010, with a total of ten reaction modules, of which the 1st to 5th reaction modules are the first reaction area, the 6th to 10th reaction modules are the second reaction area, A channel and B channel are connected with the first The reaction modules are connected, and the C channel is connected to the sixth reaction module; the liquid holding capacity of each reaction module is 0.75mL, and the liquid holding capacity of the pipeline and joint is 2.9mL; the infusion pump model: PF100 semi-preparative medium-pressure infusion pump.

[0043] (1) Control the temperature of the first reaction zone and the second reaction zone to be -2°C;

[0044] (2) Place 710 g of hydrochloric acid solution with 100 g of 2,3-dimethylaniline in the storage bottle of channel A; place 180 g of aqueous solution of 70 g of sodium nitrite in the storage bottle of channel B; The ...

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Abstract

The invention relates to a continuous synthesis method of 2, 3-dimethyl phenyl dimethyl sulfide, and belongs to the technical field of fine chemical engineering. According to the method, a micro-channel reactor is used as reaction equipment, a channel A is a hydrochloric acid solution of 2, 3-dimethylaniline, a channel B is a sodium nitrite solution, and a channel C is a sodium methyl mercaptide solution; the method comprises the following steps: reacting substances in a channel A and a channel B in a first reaction zone, and then reacting an obtained reaction solution with substances in a channel C in a second reaction zone to obtain a reaction solution containing 2, 3-dimethylphenylmethyl sulfide. According to the method, the continuous production of synthesizing the 2, 3-dimethylphenylsulfide by taking the 2, 3-dimethylaniline as the raw material is realized, the operation process is simplified, the production cost is reduced, and the safety of subsequent production is improved.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a continuous synthesis method of 2,3-dimethylanisole. Background technique [0002] 2,3-Dimethylanisole is an important intermediate in the synthesis of the corn post-emergence herbicide fenflumezone, and is also used in the synthesis of other pesticides and medicines. The reported synthetic methods can be divided into 2,3-dimethylbromobenzene method and 2,3-dimethylaniline method according to the raw materials. [0003] Disclosed in the patent CN1443180A is a method for preparing 2,3-dimethylanisole sulfide, which uses 2,3-dimethylaniline as a raw material, first diazotized with sodium nitrite, and the pH is controlled at 2- 3, and then react with ethyl potassium xanthate and methyl iodide to form 2,3-dimethylanisole with a yield of about 78%. The raw materials of this method are easy to obtain, but the operation process is cumbersome, there are many "three wastes", and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/14C07C319/28C07C321/28
Inventor 仝亚飞刘顺领陈广赟王慧赵文静
Owner 山东亿盛实业股份有限公司
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