Method of preparing amide from ketoximes by Beckmann rearrangement

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

Inactive Publication Date: 2007-02-28
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 1-15

[0022] The sulfonyl chloride functionalized ionic liquid used in the embodiment of the present invention, ketoxime, the amount of ketoxime, the molar ratio of ketoxime to ionic liquid, the reaction time, the reaction temperature, the product amide and the conversion rate of ketoxime and the product amide after the reaction The selectivity is listed in Table 1.

[0023] Reality

apply

example

Ionic liquid (mmol)

reactant ketoxime

(mmol)

Ketoxime / ion

the liquid

(mol / mol)

Reaction temperature

degree(℃)

when reacting

room (h)

product

Amide

Ketoxime

conversion rate

(%)

Amide selection

selectivity

(%)

1

3-Methyl-1-(4-chlorosulfur

Acylbutyl) imidazolium trifluoride

Methanesulfonate (5)

Cyclohexanone oxime

(5)

1 / 1

80 ...

Embodiment 16

[0027] The experimental procedure is the same as in Example 1. After the reaction, extract the product with 15ml of ether for 3 times, extract the volatile matter from the extracted ionic liquid at 100°C and 5mmHg vacuum for 30 minutes, then add 5mmol of cyclohexanone oxime to it, and investigate the catalytic reaction under the same conditions as above. System cycle usage. The conversion rate of cyclohexanone oxime was 96.3% during the first recycling, and the selectivity of caprolactam was 94.2%; the conversion rate of cyclohexanone oxime was 88.6% during the second recycling, and the selectivity of caprolactam was 92.5%; The conversion rate of cyclohexanone oxime was 69.1% and the selectivity of caprolactam was 58.7% during the third recycling.

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PUM

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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: possessing indoor ionic liquid with chlorosulfonylation functional group as reacting dielectric; transmitting into functional group under mild reacting temperature and shorter reacting time; recycling the ionic liquid catalytic system.

Description

technical field [0001] The invention relates to a method for preparing amide through Beckmann rearrangement reaction of ketoxime. Background technique [0002] Room temperature ionic liquid (RTIL) refers to salts 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 100°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 polarity and no coordination; (3) ionic liquids and Non-polar organic solvents are insolub...

Claims

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Application Information

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Patent Type & Authority Applications(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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