Method for repapering sulfoxide catalyst and selectively preparing sulfoxide compound

A catalyst and sulfoxide-based technology, applied in the preparation of organic compounds, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of low reaction selectivity, complex process, low catalyst activity, etc., and achieve product selectivity High, easy to separate, easy to recycle and reuse

Active Publication Date: 2018-05-04
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In short, most of the current methods for selective oxidation of sulfides have defects such as low catalyst activity, low reaction selectivity, and complicated processes.

Method used

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  • Method for repapering sulfoxide catalyst and selectively preparing sulfoxide compound
  • Method for repapering sulfoxide catalyst and selectively preparing sulfoxide compound
  • Method for repapering sulfoxide catalyst and selectively preparing sulfoxide compound

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preparation example Construction

[0035] The preparation method of the nano-silica supported imidazole ionic liquid catalyst of one embodiment, comprises the following steps:

[0036] (1) Imidazole (0.5mol) and 3-chloropropyltriethoxysilane (0.55mol) were reacted in toluene (600mL) solvent at 110°C for 22 hours, then added triethylamine (0.5mol) and continued to react for 2 hours , recover the solvent and dry to obtain intermediate 1,

[0037] (2) Then intermediate 1 (0.3mol) and 1-bromobutane (0.33mol) were reacted in toluene (300mL) at 90°C for 10 hours, the solvent was recovered and dried to obtain intermediate 2,

[0038] (3) Intermediate 2 (0.04mol) reacted with nano-silica (13g) in toluene (200mL) at 110°C for 24 hours, filtered, and dried ionic liquid 3,

[0039] (4) Ionic liquid 3 (5g) is mixed with ferric chloride (0.01mol), cupric chloride (0.01mol), cuprous chloride (0.01mol) or cobalt chloride (0.01mol) in acetonitrile (100mL) solvent Reaction at 70°C for 24 hours,

[0040] (5) Filtration, washi...

Embodiment 1

[0043] In the reaction flask, add sulfide anisole (0.1mol), supported ionic liquid nano-SiO 2 @IL[FeCl 3 Br] (0.4g), MIL-53(Fe) (0.12g), hydrogen peroxide (0.11mol) was slowly added under stirring, and the stirring reaction was continued at 35°C for 2 hours. Cool and filter to recover the catalyst. The results of LC-MS analysis showed that the conversion rate of sulfide anisole was 98.6%, and the selectivity of sulfoxide was 89.3%.

Embodiment 2

[0045] In the reaction flask, add sulfide anisole (0.1mol), supported ionic liquid nano-SiO 2 @IL[FeCl 3 Br] (0.4g), MIL-53(Cr) (0.12g), hydrogen peroxide (0.11mol) was slowly added under stirring, and the stirring reaction was continued at 30°C for 2 hours. Cool and filter to recover the catalyst. The results of LC-MS analysis showed that the conversion rate of sulfide anisole was 97.2%, and the selectivity of sulfoxide was 98.7%.

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Abstract

The invention relates to a production process for preparing a sulfoxide compound through selective oxidation of sulfur ether. According to the particular production process, the sulfoxide compound isprepared from sulfur ether through high-selectivity oxidation reaction in a mild reaction system by taking hydrogen peroxide as an oxidizing agent under a synergic catalytic effect of nano-silica supported ionic liquid and a metal-organic framework material (MOFs). A catalyst disclosed by the invention is easy to prepare, can be well recycled and repeatedly used and is high in chemical selectivity, and a preparation method is mild in reaction conditions, simple in operation and high in oxidation rate and is an efficient, clean and environment-friendly method.

Description

technical field [0001] The invention relates to a new method for preparing sulfoxide compounds by catalyzing the selective oxidation of sulfides by loaded ionic liquids and metal-organic framework materials (MOFs), and belongs to the technical field of chemical engineering. technical background [0002] Sulfoxide compounds are very important chemical products and are widely used in the synthesis of pharmaceuticals, pesticides and other compounds. At present, the common method for producing sulfoxides is the selective oxidation of thioethers. The traditional method uses stoichiometric oxidants, such as hypochlorite, periodiodine reagent, N-bromosuccinimide, nitrate and organic peroxide, etc. However, these methods have low oxidation selectivity and make thioether Excessive oxidation into sulfone, while there are many other by-products, product separation is difficult, the utilization rate of atoms is low, and post-processing will produce environmentally harmful waste, which ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02B01J31/30C07C315/02C07C317/14C07C317/04B01J31/22
CPCB01J31/0284B01J31/0295B01J31/1691B01J31/30B01J35/0006B01J2231/70B01J2531/62B01J2531/842C07C315/02C07C317/14C07C317/04Y02P20/584
Inventor 胡玉林谭津姚楠马斌
Owner CHINA THREE GORGES UNIV
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