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A kind of method utilizing microchannel reactor to prepare sulfoxide or sulfone

A micro-channel reactor, sulfoxide technology, applied in chemical instruments and methods, organic chemistry methods, preparation of organic compounds, etc., can solve the problems of low product yield, poor purity, long reaction time, etc.

Active Publication Date: 2016-06-08
LIANHE CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the long reaction time and high risk of reaction in the preparation method of sulfoxide or sulfone in the prior art, which is not suitable for the preparation of kilogram-level products, cannot be continuously produced, and has poor selectivity between sulfoxide and sulfone , low product yield, poor purity, and not suitable for large-scale industrial production, and a method for preparing sulfoxide or sulfone using a microchannel reactor is provided

Method used

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  • A kind of method utilizing microchannel reactor to prepare sulfoxide or sulfone
  • A kind of method utilizing microchannel reactor to prepare sulfoxide or sulfone
  • A kind of method utilizing microchannel reactor to prepare sulfoxide or sulfone

Examples

Experimental program
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Effect test

Embodiment 1

[0041]

[0042] 1. Raw material preparation: Weigh 100.0 grams of 2-(isopropylsulfide)nitrobenzene, pour it into a container containing 300.0 grams of acetic acid, stir to make it evenly mixed, and then seal it. Then weigh 126.4 grams of hydrogen peroxide with a mass percentage of 30% (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

[0043] 2, utilize the device of the present invention figure 2 , according to the following steps: (1) the acetic acid solution containing 2-(isopropylsulfide) nitrobenzene in the raw material tank 1 enters the Corning microchannel 7 through the raw material pump 3, and the oxidant 30% hydrogen peroxide in the raw material tank 2 passes through the raw material pump 4 enter Corning microchannel 7; (2) adopt continuous flow microchannel reactor in the reaction process, the acetic acid solution of raw material 2-(isopropylsulfide g...

Embodiment 2

[0046]

[0047] 1. Raw material preparation: Weigh 100.0 grams of 2-(isopropylsulfide)nitrobenzene, pour it into a container containing 300.0 grams of acetic acid, then add 1.0 grams of concentrated sulfuric acid dropwise to the container at room temperature, and stir Mix well and seal. Then weigh 126.4 grams of hydrogen peroxide with a mass percentage of 30% (the mass percentage refers to the percentage of the mass of hydrogen peroxide in the total mass of hydrogen peroxide), place it in another container, and seal it.

[0048] 2, utilize the device of the present invention figure 2 , according to the following steps: (1) the acetic acid solution containing 2-(isopropylsulfide group) nitrobenzene and concentrated sulfuric acid in the raw material tank 1 enters the Corning microchannel 7 through the raw material pump 3, and the oxidant mass percentage in the raw material tank 2 is 30% hydrogen peroxide (the mass percentage refers to the percentage that the quality of hydr...

Embodiment 3

[0051]

[0052] 1. Raw material preparation: Weigh 100.0 g of dimethyl sulfide, place it in a container and seal it, pour it into a container containing 300.0 g of acetic acid, stir to make it evenly mixed, and then seal it. Then weigh 401.4 grams of 30% hydrogen peroxide, place it in another container, and seal it.

[0053] 2. Use figure 2 The device diagram of the present invention, according to the following steps: (1) dimethyl sulfide in the raw material tank 1 enters the microchannel reaction 7 through the raw material pump 3, and the oxidant mass percentage in the raw material tank 2 is 30% hydrogen peroxide (the described quality Percent means that the quality of hydrogen peroxide accounts for the percentage of the total mass of hydrogen peroxide) enters Corning microchannel 7 through raw material pump 4; (i.e. 100.0 grams of 2-methyl sulfide: 401.4 grams of 30% hydrogen peroxide feed), mixed reaction at a set temperature of 50°C; (3) controlled by adjusting the fl...

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Abstract

The invention discloses a method for preparing sulfoxide and sulfone by utilizing a microchannel reactor. The invention provides a method for preparing sulfoxide or sulfone, which comprises the following steps: the homogeneous solution formed by thioether 1 and a solvent, and the oxidizing agent are injected into a microchannel reactor through a metering pump respectively, contacted in the microchannel and Carry out the oxidation reaction to obtain sulfoxide or sulfone, and the time of the oxidation reaction is 1 second to 300 seconds; the preparation method of the present invention has extremely short reaction time, precise control of reaction conditions, high safety, and is suitable for kilogram-level products Rapid preparation, continuous production, high selectivity of sulfoxide and sulfone, high product yield, good purity, suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a method for preparing sulfoxide or sulfone using a microchannel reactor. Background technique [0002] Sulfoxide and sulfone are important chemical raw materials and intermediates for the synthesis of other pharmaceuticals and pesticides. They are mainly used in fine chemicals, pharmaceuticals, pesticides, synthetic fibers, plastics, printing and dyeing, rare metal extractants, and organic synthesis. Sulfoxides and sulfones are mainly used as raw materials for pharmaceuticals and other organic synthesis, and are also used in antacid and anti-ulcer drugs, ophthalmic medicines, anti-leprosy drugs, antibiotics, stimulant drugs such as armodafinil, herbicides and insecticides , Electrolyte functional additive, can also be used as raw material for engineering plastics and membrane materials. [0003] At present, sulfoxide and sulfone are prepared by the oxidation method of sulfide and nitric acid and nitrate, the synthesis method ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07B45/00C07C315/02C07C317/14C07C317/04C07C317/22C07C317/44C07D401/12
Inventor 王萍潘强彪邹本立荆琪杨优焱
Owner LIANHE CHEM TECH
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