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Chemical synthesis method for amide substance

A technology for chemical synthesis and amides, applied in the field of chemical synthesis of amides, can solve the problems of large acid consumption, easy deactivation of catalysts, and high reaction temperature, and achieves high reaction yield, low production cost, and mild reaction conditions. Effect

Inactive Publication Date: 2007-08-15
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods are seriously polluted due to the large amount of acid used, the high reaction temperature catalyst is easily deactivated, and the range of application is small (only realize industrialization in caprolactam) etc. need to be further improved

Method used

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  • Chemical synthesis method for amide substance
  • Chemical synthesis method for amide substance
  • Chemical synthesis method for amide substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The ratio of the amount of feed material to ketoxime: bis (trichloromethyl) carbonate: N, N-disubstituted amide is 3: 1: 3, ketoxime is acetophenone oxime, N, N-disubstituted amide is N, N-dimethylformamide, acetonitrile is used as a solvent, and its consumption is 6 times of the quality of bis(trichloromethyl)carbonate.

[0020] In a 150mL four-necked flask equipped with a thermometer, a reflux condenser and mechanical stirring, add 25mmol (7.4g) of bis(trichloromethyl)carbonate, dissolve it with 45g of acetonitrile, and add N,N-dicarbonate dropwise under an ice-water bath. Methylformamide 75mmol (5.5g), stirred at -5°C to 5°C for 1h, then added 75mmol (9.0g) of acetophenone oxime, heated to 85°C, and reacted at 80°C to 85°C for 2h, after the reaction was completed, Add saturated sodium carbonate solution to adjust to PH = 7, separate the organic layer, cool in an ice bath, stir for 10 minutes, filter, the filter cake is light yellow and it is crude acetanilide, after ...

Embodiment 2

[0022] The ratio of the amount of feed material to ketoxime: bis(trichloromethyl) carbonate: N, N-disubstituted amides is 3: 1.2: 3.6, and ketoxime is acetophenone oxime, and the feeding amount is 75mmol, and bis(trichloromethyl) Base) carbonate charging amount is 30mmol, N, N-disubstituted amide is N, and N-dimethylformamide charging amount is 90mmol, and acetonitrile is as organic solvent, and its consumption is 54g, i.e. two (trichloromethyl) carbonic acid 6 times the mass of the ester.

[0023] Other operations were the same as in Example 1, and the product yield of acetanilide was 90.8%, and the purity was 99.2%.

Embodiment 3

[0025] The ratio of the amount of feed material to ketoxime: bis(trichloromethyl)carbonate: N, N-disubstituted amides is 3: 1.5: 4.5, and ketoxime is acetophenone oxime, and the feeding amount is 75mmol, and bis(trichloromethyl) Base) carbonate charging amount is 37.5mmol, N, N-disubstituted amide is N, and N-dimethylformamide charging amount is 112.5mmol, and acetonitrile is as organic solvent, and its consumption is 67.5g, i.e. bis(trichloroform base) 6 times the mass of carbonate.

[0026] Other operations were the same as in Example 1, and the product yield of acetanilide was 91.1%, and the purity was 98.7%.

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Abstract

The invention discloses a chemical synthesizing method of amide material, which comprises the following steps: adopting di-(trichloromethyl)-carbonate and N, N-disubstituted amide to react in the organic solvent under -5-5 deg.c to make Vilsmeier agent; adding ketoximes under 20-150 deg.c for 1-12h; setting the molar rate of putting material of ketoximes, di-(trichloromethyl)-carbonate and N, N-disubstituted amide at 3:0.5-2:1.5-6; separating and purifying; obtaining the product with low cost.

Description

(1) Technical field [0001] The invention relates to a chemical synthesis method of amides. (2) Background technology [0002] Amide products are important chemical raw materials, dyes and pharmaceutical intermediates, and are widely used in agriculture and industry. [0003] Most of the chemical synthesis methods of amides in the prior art are prepared by acylating anilines as raw materials, and commonly used acylating agents are acid chlorides, acid anhydrides or carboxylic acids. However, such methods usually have many side reactions, high reaction temperature, long time, and easy to corrode equipment. There are also a large number of reports on the preparation of amides from ketoxime. The traditional method uses strong acid as a catalyst, such as concentrated sulfuric acid, concentrated phosphoric acid, concentrated hydrochloric acid, etc., and the gas phase rearrangement method has also been applied to industrialization. However, these methods need to be further impro...

Claims

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Application Information

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IPC IPC(8): C07C231/10C07C233/07C07D223/16
Inventor 李坚军李平苏为科
Owner ZHEJIANG UNIV OF TECH
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