Synthesis method based on amination reaction of aryl siloxane

Abstract

The invention relates to a synthesis method based on amination reaction of aryl siloxane. The method comprises the following steps: adding AgF, a reactant I, a reactant II, a butanone solution and a number 5 magneton into a reactor in sequence, connecting a condenser pipe, introducing condensate water from bottom to top, placing the reactor in an oil bath pan at 30-70 DEG C, heating, stirring and reacting for 10-12 hours, terminating the reaction, and purifying the product to obtain an aryl siloxane amination product, wherein the reactant I is optionally selected from phenyl triethoxy silane, p-tert-butyl phenyl triethoxy silane, p-methoxy phenyl triethoxy silane, p-methyl phenyl triethoxy silane, p-chlorphenyl triethoxy silane or 4-triethoxy silicon biphenyl; and the reactant II is diethyl azodicarboxylate. The method is mild in reaction condition, high in selectivity, relatively high in yield and environment-friendly; and the compound has certain biological activity and can be used in the field of synthesis of drugs, pesticides and paint dyes.

Description

technical field [0001] The invention relates to a synthesis method for the amination reaction of aryl siloxanes, in particular to a synthesis method for realizing C-N coupling through aryl siloxane compounds. Background technique [0002] Amine compounds are important chemical intermediates and products, which are widely used in the fields of medicine, pesticides, coatings, analytical reagents and dyes. For example: a series of triptan compounds such as fluvatriptan, naratriptan, sumatriptan and almotriptan, which are an important class of drugs used to treat migraine, mostly use phenylhydrazine hydrochloride as an intermediate Another example is the use of phenylhydrazine as an analytical reagent to identify carbonyl-containing compounds such as aldehydes, ketones, and sugars. The application of these amine compounds also makes the research on the synthesis of amine compounds more practical. [0003] There are many synthetic methods of amine compounds, such as the aminatio...

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Problems solved by technology

[0003] There are many synthetic methods of amine compounds, such as the amination reaction of arylboronic acid compounds, although this type of reaction is the main method for the synthesis of amine compounds reported recently One of the methods, but there are certain limitations in its reaction conditions, such as: expensive catalyst used, poor applicability, dangerous preparation conditions, environmental pollution, etc.; another preparation of amine compounds is the amination reaction of halogenated aryl groups. The reaction uses copper salt as a catalyst, but dangerous reagents such as NaH need to be added as an auxiliary reagent for the reaction; although the required amine compounds can be effectively synthesized, the post-treatment process of the experiment is quite dangerous and the solvent DMF used is residual. The generated waste water or waste gas pollute the environment very seriously

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