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Method of preparing amide from ketoximes by Beckmann rearrangement

A Beckmann rearrangement, ketoxime technology, applied in the preparation of carboxylic acid amides, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of low value-added ammonium sulfate, difficult heat transfer, severe reaction heat release, etc. To achieve the effect of simple treatment, good selectivity and simple reaction system

Inactive Publication Date: 2008-03-12
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

(1) A large amount of low-value-added ammonium sulfate (4.2-4.6t / t caprolactam) is produced as a by-product; (2) The equipment is severely corroded; (3) The reaction is exothermic and heat transfer is difficult; (4) A large amount of acidic wastewater is produced to cause environmental pollution Pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-14

[0022] Acyl chlorides used in Examples 1-14 of the present invention, room temperature ionic liquid, ketoxime, the amount of ketoxime, the molar ratio of ketoxime to ionic liquid, reaction time, reaction temperature, product amide and the conversion rate of ketoxime after the end of the reaction and The selectivities of the product amides are listed in Table 1.

[0023] Table 1 Ketoxime prepares the method embodiment of amide through Beckmann rearrangement reaction

[0024] Reality

apply

example

Ionic liquid (mmol)

Acid chloride

(mmol)

Ketoxime

(mmol)

Acyl chloride / ketoxime /

ionic liquid

The molar ratio of

reaction

temperature

(℃)

reaction

time

(h)

Product amide

Conversion rate

(%)

selectivity

(%)

1

1-Butyl-3-methylimidium

...

Embodiment 15

[0030] Experiment material and reaction condition are identical with embodiment 6. After the reaction, the product was extracted three times with 15ml of water, and the remaining ionic liquid system was vacuumed at 100°C and 5mmHg for 30 minutes to remove volatile matter, then 5mmol of cyclohexanone oxime was added to it, and the reaction was carried out under the same conditions as above. The catalytic system was reused. Condition. The result shows that the conversion rate of cyclohexanone oxime is 84.9% when using for the first time, and the selectivity of caprolactam is 97.3%; %.

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Abstract

The invention discloses an amide preparing method of indoor temperature ionic liquid catalytic ketoximes through Beckmann rearrangement reaction, which is characterized by the following: selecting catalyst from acylated-chloride compound; transmitting into amide under mild reacting temperature and shorter reacting time; extracting product through water; recycling the ionic liquid catalytic system.

Description

technical field [0001] The invention relates to a method for preparing amide through Beckmann rearrangement reaction of ketone oxime catalyzed by acid chloride compound in room temperature ionic liquid. Background technique [0002] Room temperature ionic liquid (RTIL) refers to salts that are mainly composed of organic cations and inorganic or organic anions that are liquid at room temperature or near room temperature, and their melting point is generally less than 150 °C. Compared with traditional organic solvents, water and supercritical fluids, they have many incomparable unique properties, mainly in the following aspects: (1) Ionic liquids are excellent solvents for many organic, inorganic and polymer materials, with low viscosity and high thermal conductivity. Large capacity, most of them can be homogeneously mixed in any proportion; (2) ionic liquids are usually composed of ions that are difficult to coordinate with other compounds, so they can be solvents with high p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/10
Inventor 邓友全杜正银李作鹏
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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