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Method for synthesizing benzamide compounds by electro-catalysis in aqueous phase at room temperature

A technology of benzamide and electrocatalysis, applied in electrolysis process, electrolysis components, electrolysis organic production and other directions, can solve the problems of producing many by-products, long reaction time, etc., and achieves a solution with few by-products, easy operation and high yield. Effect

Inactive Publication Date: 2019-02-19
FUJIAN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods often use toxic solvents, precious metals, expensive microwave reactors and highly toxic chlorinated reagents, and the operation is complicated and needs to be carried out under anhydrous and oxygen-free conditions, resulting in many by-products and long reaction times. The leap from small-scale synthesis of formamide compounds to large-scale industrial synthesis

Method used

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  • Method for synthesizing benzamide compounds by electro-catalysis in aqueous phase at room temperature
  • Method for synthesizing benzamide compounds by electro-catalysis in aqueous phase at room temperature
  • Method for synthesizing benzamide compounds by electro-catalysis in aqueous phase at room temperature

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Embodiment 1: benzamide: add benzoic acid 1 mmol, 25-28% ammoniacal liquor 2 ml, cesium carbonate 0.2mmol and 0.01mmol tetrabutylammonium bromide in the flask, use Pt-Pt electrode to pass into 20 under the condition of room temperature The mA current was reacted for 20 min, concentrated under reduced pressure, and the product was recrystallized from ethanol to obtain a white solid with a yield of 98%.

Embodiment 2

[0028] Example 2: N -Methylbenzamide: Add 1 mmol of benzoic acid, 1 mmol of methylamine, 2 ml of water, 0.2 mmol of cesium carbonate and 0.01 mmol of tetrabutylammonium bromide in a flask, and use a Pt-Pt electrode to feed 20 The mA current was reacted for 20 min, concentrated under reduced pressure, and the product was recrystallized from ethanol to obtain a white solid with a yield of 97%.

Embodiment 3

[0029] Example 3: N -Ethylbenzamide: the preparation method is the same as in Example 2, the electrode adopts Pt-Ag electrode instead of Pt-Pt electrode, methylamine is replaced by ethylamine, and a white solid is obtained with a yield of 97%.

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Abstract

The invention discloses a method for synthesizing benzamide compounds by electro-catalysis in an aqueous phase at room temperature. A constant current is used for giving energy, benzoic acid and amineare substituted in the aqueous phase for coupled reaction, and the method for preparing the benzamide compounds is environmentally friendly, simple and convenient to operate, safe and cheap and efficient. Compared with the prior art, the method can apply to a large number of functional groups, has high yield and less by-products, and is simple to operate, safe, low in cost, and capable of achieving environmental protection; and Please see the description for the formula.

Description

technical field [0001] The invention belongs to a method for simply utilizing electrocatalysis to synthesize benzamide compounds in water phase at room temperature. Background technique [0002] Benzamide is a common intermediate in the synthesis of heterocyclic compounds. It also has some physiological activities and can be used as herbicides, fungicides, dispersants, antipsychotics and vasodilators. It can be said that benzamide compounds is very important. At present, the main methods of synthesizing benzamide compounds reported in the literature are: (1) synthesis using metal catalysts in a solvent; (2) microwave synthesis; (3) two-step synthesis. These methods often use toxic solvents, precious metals, expensive microwave reactors and highly toxic chlorinated reagents, and the operation is complicated and needs to be carried out under anhydrous and oxygen-free conditions, resulting in many by-products and long reaction times. The leap from a small amount of synthesis ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/00
CPCC25B3/00
Inventor 柯方许贻文王津张鹏林媚陈艳周孙英
Owner FUJIAN MEDICAL UNIV
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