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Method for photocatalytic synthesis of disulfide in water phase

A technology for disulfide compounds and synthesis methods, which is applied in the preparation of hydrogenated polysulfides/polysulfides, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of high cost, low conversion and selectivity, and high energy cost

Active Publication Date: 2021-08-10
NANYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although there are many systems for catalytically preparing disulfide compounds, there are also some unsatisfactory problems: (1) low conversion and selectivity; (2) use of toxic organic solvents; (3) complex synthesis of catalysts and low cost High; (4) High energy cost

Method used

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  • Method for photocatalytic synthesis of disulfide in water phase
  • Method for photocatalytic synthesis of disulfide in water phase

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Effect test

Embodiment 1

[0015] Embodiment 1 of a method for photocatalytically synthesizing disulfide compounds in an aqueous phase of the present invention is synthesized by the following method:

[0016] Bi 4 o 5 Br 2 / Fe 3 o 4 Add 15 mg of catalyst and 75 mg of benzyl mercaptan to 1 mL of water, mix and stir at room temperature, and irradiate with 30W blue LED for 1-3 hours. After the reaction was finished, extract with ethyl acetate solvent, use gas chromatography internal standard method to detect conversion rate and selectivity, conversion rate 97%, selectivity 93%,

[0017] .

Embodiment 2

[0018] Embodiment 2 of a method for photocatalytically synthesizing disulfide compounds in an aqueous phase of the present invention is synthesized by the following method:

[0019] Bi 4 o 5 Br 2 / Fe 3 o 4 Add 15 mg of catalyst and 75 mg of cyclohexanethiol into 1 mL of water, mix and stir at room temperature, and irradiate with 30W blue LED for 1-3 hours. After the reaction, extract with ethyl acetate solvent, use gas chromatography internal standard method to detect conversion rate and selectivity, conversion rate 98%, selectivity 98%,

[0020] .

Embodiment 3

[0021] Embodiment 3 of a method for photocatalytically synthesizing disulfide compounds in an aqueous phase of the present invention is synthesized by the following method:

[0022] Bi 4 o 5 Br 2 / Fe 3 o 4 Add 15 mg of catalyst and 75 mg of 1-pentanethiol into 1 mL of water, mix and stir at room temperature, and irradiate with 30W blue LED for 1-3 hours. After the reaction was finished, extract with ethyl acetate solvent, use gas chromatography internal standard method to detect conversion rate and selectivity, conversion rate 93%, selectivity 96%,

[0023] .

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Abstract

The method comprises the following steps: mixing a catalyst Bi4O5Br2 / Fe3O4 with the mass percent of 10-20% and mercaptan in 1-5 mL of water, irradiating for 1-3 hours by adopting a 30W blue light LED under the condition of room temperature in the air, performing extracting by using an ethyl acetate solvent after the reaction is finished, and detecting the conversion rate and selectivity by using a gas chromatography internal standard method, wherein the conversion rate is greater than 90%, and the selectivity is greater than 90%. According to the method, a magnetic recoverable composite catalyst Bi4O5Br2 / Fe3O4 is used, water is taken as a solvent, mercaptan coupling oxidation is carried out at room temperature to prepare the disulfide, the catalyst can be recycled through magnetic control after the reaction is finished, and benzyl mercaptan can be converted into the disulfide within 2 hours at room temperature in a water phase.

Description

technical field [0001] The invention relates to the synthesis of compounds, in particular to a method for photocatalytically synthesizing disulfide compounds in water phase, which is a method for preparing disulfide compounds from photocatalyzed thiol compounds in water phase. Background technique [0002] Coupling reactions are an essential process in organic synthesis and have a wide range of applications in the fields of chemistry, medicine, biology, and materials. Among them, the selective coupling of sulfhydryl groups to disulfide compounds is a very important and classic type. Disulfides have been shown to protect against oxidative damage in biological systems, play a role in protein folding and microtubule assembly in vitro, and have been studied as drug delivery systems. Rubber and elastomers can be imparted with excellent tensile strength by disulfide compounds. Some recent studies have shown that disulfide compounds are bactericidal and protect against cyanide po...

Claims

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Application Information

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IPC IPC(8): C07C319/24C07C321/20C07C321/22C07C321/14C07C323/07B01J27/128
CPCC07C319/24B01J27/128C07C2601/14B01J35/39B01J35/33C07C321/20C07C321/22C07C321/14C07C323/07Y02P20/584
Inventor 杨春霞赵伟
Owner NANYANG NORMAL UNIV
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