The preparation method of trifluoroalkyl sulfone compound

A technology of trifluoroalkyl sulfone and trifluoroalkyl sulfide, which is applied in the field of preparation of trifluoroalkyl sulfone compounds, can solve problems such as the decomposition of hydrogen peroxide, and achieve the effects of reducing decomposition, reducing synthesis costs, and reducing the amount of materials

Active Publication Date: 2020-05-26
ASYMCHEM LIFE SCI TIANJIN
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Problems solved by technology

[0007] The main purpose of the present invention is to provide a preparation method of trifluoroalkyl sulfone compounds to solve the problem of hydrogen peroxide decomposition in the prior art when hydrogen peroxide is used as an oxidant to prepare trifluoroalkyl sulfone compounds

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  • The preparation method of trifluoroalkyl sulfone compound

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[0042] In one embodiment of the present application, the above-mentioned preparation method includes: continuously feeding the first solution containing trifluoroalkyl sulfide compounds, the aqueous solution containing sodium tungstate dihydrate, and the hydrogen peroxide solution into a continuous reactor respectively .

[0043] In this application, the above-mentioned trifluoroalkyl sulfide compounds and sodium tungstate dihydrate are made into solutions in advance, and then respectively sent into continuous reactors, which is beneficial to the trifluoroalkyl sulfide compounds, tungsten Sodium dihydrate is uniformly dissolved in the solution to form a homogeneous reaction system in the continuous reactor. On the one hand, it helps the above three materials to disperse more uniformly under the same reaction conditions, thereby increasing the probability of collision between the molecules of the reaction materials, thereby improving the efficiency of the reaction; on the other...

Embodiment 1

[0053] Control the temperature at 15-25 ℃, and prepare the following materials respectively: Dissolve trifluoromethyl phenylene sulfide (A, 30 g, 0.168 mol) in acetonitrile (270 mL) and stir to clarify, which is recorded as material 1; Na 2 WO 4 2H 2 O (5.10 g, 0.015 mol) was dissolved in distilled water (5.4 mL) and stirred to clarify, which was recorded as material 2; 35% H 2 o 2 (81.62 g, 0.84 mol) was recorded as material 3; the retention volume of the continuous coil was 100 mL, and the retention time of the reaction system in the coil was controlled to be 60 min.

[0054] Before feeding, the coil temperature is controlled at 50 °C, and the above-mentioned material 1, material 2 and material 3 are continuously injected into the coil in proportion by using a plunger pump. Among them, the feeding speed of material 1 is 4.06 g / min, the feeding speed of material 2 is 0.18 g / min, and the feeding speed of material 3 is 1.36 g / min. The three materials are fed at the same time...

Embodiment 2

[0056]Control the temperature at 15-25 °C, and prepare the following materials respectively: Dissolve p-chlorotrifluoromethylphenylsulfide (A, 35.72 g, 0.168 mol) in acetonitrile (321.5 mL) and stir to clarify, which is designated as material 1; Na 2 WO 4 2H 2 O (5.10 g, 0.015 mol) was dissolved in distilled water (6.43 mL) and stirred to clarify, which was recorded as material 2; 35% H 2 o 2 (81.62 g, 0.84 mol) was recorded as material 3; the retention volume of the continuous coil was 100 mL, and the retention time of the control reaction system in the coil was 60 min.

[0057] Before feeding, the coil temperature is controlled at 50 °C, and the above-mentioned material 1, material 2 and material 3 are continuously injected into the coil in proportion by using a plunger pump. Among them, the feeding speed of material 1 is 4.83 g / min, the feeding speed of material 2 is 0.19 g / min, and the feeding speed of material 3 is 1.36 g / min. The three materials are fed at the same ti...

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Abstract

The invention provides a preparation method of trifluoroalkyl sulfone compounds. The preparation method comprises that trifluoroalkyl sulfide compounds, sodium tungstate dihydrate and hydrogen peroxide solution are continuously fed into a continuous reactor through feeding equipment, so that the trifluoroalkyl sulfide compounds undergo oxidation reactions to obtain The product system of hydrocarbyl sulfone compounds, wherein the trifluorohydrocarbyl sulfide compound has the structure shown in the structural formula, and R is any one of the following groups: straight-chain alkyl, branched-chain alkyl, substituted aryl, non- For substituted aryl, substituted heterocyclic aryl, unsubstituted heterocyclic aryl, unsubstituted cyclic alkyl and substituted cyclic alkyl, the oxidation reaction temperature is 25~50°C. This application utilizes continuous feed to improve the material contact effect, and then the oxidation reaction of thioether can be carried out at a lower temperature; and the reduction of oxidation reaction temperature effectively reduces the decomposition of hydrogen peroxide, and reduces the need for continuous pressure requirements of the reactor.

Description

technical field [0001] The invention relates to the technical field of synthesis of trifluoroalkyl sulfone compounds, in particular to a preparation method of trifluoroalkyl sulfone compounds. Background technique [0002] In recent years, since compounds containing trifluoromethyl sulfone groups are widely used in the fields of drugs, bioactive compounds, catalysts and functional materials, and have broad application prospects, the synthesis of compounds containing trifluoromethyl sulfone groups has become more and more popular. It is of great significance to develop a high-efficiency and low-cost synthesis process that has attracted more and more attention from synthetic workers. [0003] At present, the industrial production of trifluoromethyl sulfone compounds is mainly obtained through the oxidation of trifluoromethyl sulfide. And the most commonly used oxidizing agent of the oxidation of trifluoromethyl sulfide is potassium permanganate and chromium trioxide, but beca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/64C07D207/36C07D213/71C07C315/02C07C317/04C07C317/08C07C317/12C07C317/14C07C317/22C07C317/24B01J23/30B01J19/00
CPCB01J19/004B01J19/0046B01J23/30B01J2219/00058B01J2219/00162B01J2219/00186C07B2200/07C07C315/02C07D207/36C07D213/71C07D307/64C07C2601/02C07C2601/14C07C317/04C07C317/08C07C317/12C07C317/14C07C317/22C07C317/24
Inventor 洪浩卢江平包登辉王学智
Owner ASYMCHEM LIFE SCI TIANJIN
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