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A kind of method for preparing amide compound

A technology of amide compounds and compounds, which is applied in the field of organic compound preparation, can solve problems such as difficult control of the progress of the reaction, and achieve the effects of simple and controllable preparation process, improved efficiency, and high efficiency

Inactive Publication Date: 2016-03-30
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Under alkaline conditions, the hydrogen peroxide oxidation method can hydrolyze nitriles into amides in a short period of time at room temperature; but this method is usually not easy to control the progress of the reaction, and the cyano group is completely hydrolyzed into carboxylic acid

Method used

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  • A kind of method for preparing amide compound
  • A kind of method for preparing amide compound
  • A kind of method for preparing amide compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolve 2-cyanopyridine (10mmol, 1.04g), NaOH (0.1mmol, 4mg) in a mixed solvent of toluene / water (V:V=3:1), reflux for 6 hours, stop the reaction, and let stand After room temperature, the solvent was spin-dried, purified and separated by silica gel column chromatography to obtain 0.95 g of white solid 2-amidopyridine (yield: 78%); Ms (M / Z): 122.0 (M + ).

Embodiment 2

[0032] 2-cyanopyridine (10mmol, 1.04g), K 2 CO 3 (0.5mmol, 69mg) was dissolved in a mixed solvent of toluene / water / ethanol (V:V:V=6:2:1), and after 12 hours of reflux reaction, the reaction was stopped, and after standing at room temperature, the solvent was spin-dried , Utilize silica gel column chromatography to obtain white solid 2-amidopyridine 1.04g (yield: 85%) after purifying and separating; Ms (M / Z): 122.0 (M + ).

Embodiment 3

[0034] Dissolve 2-bromo-5-cyanopyridine (10mmol, 1.83g), sodium tert-butoxide (0.1mmol, 9.6mg) in a mixed solvent of xylene / ethanol (V:V=3:1), and reflux the reaction After 4 hours, the reaction was stopped, and after standing at room temperature, the solvent was spin-dried, purified and separated by silica gel column chromatography to obtain 1.84 g of white solid 2-bromo-5-amide pyridine (yield: 92%); Ms( M / Z):201.0(M + ).

[0035] The structural formula of above-mentioned 2-bromo-5-amide pyridine is:

[0036] .

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Abstract

The invention belongs to the field of organic compound preparation, and in particular relates to a method for preparing amide compounds. Specifically, under heating conditions, the mixed solvent of protic solvent and aprotic solvent is used as the reaction medium, and the corresponding amide compound is efficiently prepared by selective hydrolysis of the cyano compound under air atmosphere and basic catalytic conditions; at the same time, it can also Further utilizing the carbon-carbon coupling reaction, the coupled amide compound can be prepared in one step by selecting a compound containing both a cyano group and a halogen group to react with a boric acid compound. The method avoids the use of traditional hydrogen peroxide and other toxic and harmful oxidants, and is a simple, efficient, green and environment-friendly synthesis method for preparing amide compounds.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, and in particular relates to a method for preparing amide compounds. Background technique [0002] Amide compounds are an important class of chemical raw materials, which are widely used in the fields of biology, medicine, and pharmacy. There are two ways to prepare amide compounds in the prior art: one is to prepare amides through the condensation reaction of carboxyl and amino groups, but this reaction usually requires activation of raw materials, and the reaction conditions are usually relatively harsh. [0003] In addition, amide compounds are prepared by hydrolysis of cyano group, which is mainly divided into hydrolysis of cyano group under acidic or alkaline conditions. Under alkaline conditions, the hydrogen peroxide oxidation method can hydrolyze nitriles to amides in a short period of time at room temperature; but this method is usually not easy to control the progress of the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/81
CPCC07C231/06C07D213/81C07C233/11C07C233/65
Inventor 周宇扬王筱梅叶常青朱赛江徐鹏杰梁作芹
Owner SUZHOU UNIV OF SCI & TECH
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