A kind of preparation method of nitrogen heterocyclic sulfide and its purification method

A technology of sulfide and nitrogen heterocycle, applied in the field of preparation of nitrogen-containing heterocycle sulfide, can solve problems such as unfavorable industrialization popularization, complex cobalt complex, expensive structure, etc., and achieves cheap synthesis system, simple process flow and cost low effect
CN107698558BActive Publication Date: 2019-04-02WENZHOU UNIVERSITY
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
WENZHOU UNIVERSITY
Publication Date
2019-04-02

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Abstract

The invention discloses a preparation method and a purification method of heterocyclic nitrogen sulfides. The preparation method includes the steps: taking N-pyridyl pyrrole or pyridyl indole and disulfide ether as substrates, taking dimethyl sulfoxide as solvents, performing heating reaction on the N-pyridyl pyrrole or pyridyl indole, the disulfide ether and the dimethyl sulfoxide under catalysisof transition metal copper salt and the action of a ligand in the air environment to prepare crude products, and performing filtration and solvent removal on the crude products to obtain remainders;performing silica column chromatography on the remainders, spraying and washing the remainders by the aid of eluting liquid, collecting effluents, combining the effluents containing products, performing concentration and solvent removal on the combined effluents, and performing vacuum drying to obtain a target product. The preparation method has the advantages of simple technological process, lowcost and high yield.
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Description

technical field

[0001] The invention belongs to the technical field of organic synthesis, in particular to a preparation method of nitrogen-containing heterocyclic sulfides and a purification method thereof. Background technique

[0002] Nitrogen heterocyclic sulfides are an important class of organic compounds with good biological activities, such as insecticidal, bactericidal, herbicidal, anti-tumor and anti-hypertensive, etc., and have played an increasingly important role in the fields of medicine and pesticides. And show good development prospects.

[0003] Literature Tobias et al. (Angew.Chem.Int.Ed.2016,55,11287-11291.) discloses the synthesis of azepines by the cobalt-catalyzed reaction of N-pyrimidinyl indole with benzenethiol and diphenyl disulfide Episulfide, the method thereof comprises a preparation process and a purification process.

[0004] 1. The preparation process is as follows:

[0005] Take N-pyrimidinyl indole as substrate (0.5mmol), add benzenethiol...

Claims

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