Method for preparing carboxylic acid compound by promoting rapid hydrolysis of cyan

A compound and carboxylic acid technology, which is applied in the field of promoting the rapid hydrolysis of cyano groups to prepare carboxylic acid compounds, can solve the problems of incomplete reaction of amides and carboxylic acids, harsh reaction conditions, and large amount of acid, and achieve easy implementation and reaction The effect of low temperature and simple process

Inactive Publication Date: 2011-06-15
TIANJIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Amide derivatives can be prepared under metal ions and acid and alkali conditions, but when hydrolyzing carboxylic acids, the method of using low-concentration alkali or acid and adding metal ions is no longer applicable, the reaction conditions are more harsh, and the reaction is often incomplete. Mixture of amid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 2g of sodium hydroxide to 10mL of water to prepare a lye with a concentration of 16.7%; add 0.4g of sodium iodide, stir to dissolve, add 1.2g of butyronitrile, raise the temperature to reflux state under stirring, and hydrolyze for 1 hour. The solution was allowed to stand and cooled to room temperature, and gradually added sulfuric acid with a concentration of 10% under stirring. When the pH value was close to 7, a large amount of crystals were precipitated, and neutralization was stopped. After the crystals were completely precipitated, filtered to obtain sodium butyrate solid, the solid Dissolved in deionized water, neutralized with 20% hydrochloric acid to pH=5, extracted with anhydrous ether, dried, and evaporated to obtain butyric acid. Yield: 87%. Boiling point: 164°C,; Infrared spectrum data (cm -1 ): 2980, 1720, 1468, 1420, 1288.

Embodiment 2

[0021] Add 4g of potassium hydroxide to 10mL of water to prepare a lye with a concentration of 28.7%; add 1g of sodium iodide, stir to dissolve, add 1.2g of anthranil, heat up to reflux state under stirring, and after hydrolysis for 1 hour, dissolve The reaction solution was allowed to stand and cooled to room temperature, and gradually added sulfuric acid with a concentration of 10% under stirring. When the pH value was close to 4, solids were precipitated, and neutralization was stopped. After the crystals were completely precipitated, filtered to obtain crude anthranilic acid, which Deionized water recrystallized to obtain pure anthranilic acid. Yield: 90%. Melting point: 147-148°C; infrared spectrum data (cm -1 ): 3390, 3325, 2580, 1690, 1614, 1586, 1378, 1247.

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PUM

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Abstract

The invention discloses a method for preparing a carboxylic acid compound by promoting rapid hydrolysis of cyan. Under the alkaline condition, cyan undergoes a hydrolysis reaction under the catalytic action of an iodine ion-containing compound, so that the carboxylic acid compound is generated. The method comprises the following steps of: 1) dissolving an alkaline compound or carbonate in water to obtain an alkaline solution; 2) adding an iodide into the alkaline solution, stirring for dissolving, and adding a cyan compound to perform a hydrolysis reaction; 3) cooling to the room temperature, adding sulfuric acid, and filtering after crystals are fully separated out to obtain a solid; 4) dissolving the solid in deionized water, and extracting with absolute ether; and 5) drying extract liquor, and removing diethyl ether by distilling to obtain the carboxylic acid compound. The invention has the advantages of simple process, low reaction temperature, reaction in the conventional heating device, easiness in implementing, short required reaction time, yield of up to 60 to 99 percent, and great improvement on production efficiency.

Description

technical field [0001] The invention relates to a method for promoting rapid hydrolysis of cyano groups to prepare carboxylic acid compounds, which belongs to the technical field of organic synthesis methods and chemical processes. Background technique [0002] The cyano group in the cyano (-CN) compound (organic matter is called nitrile) is a strong polar group, and the π bond is easily polarized. Most nitrile compounds are chemically synthesized, and some are produced by widely existing in nature. biosynthesis of (Acta Pharmaceutica Sinica, 2001, 28(6):76-81). Cyanide groups are often contained in many industrially valuable chemicals, and nitriles are usually used as starting materials for the synthesis of a series of amines, acids and polymers, and their hydrolysis reactions are widely used in amino acids, phthalamides, carboxylic acids and their derivatives Synthesis of compounds plays an extremely important role in organic synthesis. [0003] There have been many stud...

Claims

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Application Information

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IPC IPC(8): C07B41/08C07C53/08C07C53/122C07C51/08C07C63/06C07C53/124C07C229/56C07C227/02
Inventor 张立军宋洋罗向宁黎慧韩迪
Owner TIANJIN UNIVERSITY OF TECHNOLOGY
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