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Synthetic method for amide derivatives

A technology of amide derivatives and synthesis methods, applied in the field of amide derivatives, can solve problems such as difficult separation and reuse of unreacted raw materials, strong acid corrosion of catalysts, etc., and achieve the effect of easy operation and avoiding corrosion

Inactive Publication Date: 2003-06-25
OCEAN UNIV OF CHINA
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AI Technical Summary

Problems solved by technology

The disadvantage of these synthetic methods is that the strong acid of the catalyst is extremely corrosive, and the unreacted raw materials are difficult to separate and reuse

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1.N-(4--3--) Synthetic experiment ：(I)1000ml 3 ，50.8(0.41mol)()、40.4(0.4mol)N-、200732，400ml，N2()，(30℃)7-8。(II)，H， and 。(III)50℃，，，。(IV)，，pH to 2～3，。，，，21g，25％。 Embodiment 2

[0007] Where R is a saturated or unsaturated fatty group containing 2-12 carbon atoms, such as CH 2 =CH, CH 2 =CCH 3 , CH 3 (CH 2 ) 8 , (CH 3 ) 2 CHCH=CH(CH 2 ) 4 . The ortho or meta-disubstituted benzene used is resorcinol, catechol, o-methoxyphenol, m-methoxyphenol, o-dimethoxybenzene, m-dimethoxybenzene, o-ethoxy Base phenol, m-ethoxy phenol, o-diethoxy phenol or m-diethoxy phenol. The catalyst used in the synthesis reaction is an H-type strong acid cation exchange resin, including sulfonated coal, sulfonated styrene copolymer, sulfonated phenolic resin and the like. Among them, most of the commercially available 732-type cation exchange resins are Na-type (R-Na), which must be treated with acid to become H-type before use. During treatment, weigh 200g of 732-type cation exchange resin and place it in a beaker, add 1500ml of 3mol / L hydrochloric acid solution, soak for 1 to 2 days, pour out the upper layer, replace it with fresh 3mol / L hydrochloric acid solution, and soak for 1~...

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Abstract

The synthesis process of amide derivative includes the reaction between N-methylol fatty amide with the structure of RCONHCH2OH and benzene substitute in the presence of catalyst and inside ethanol or aceitc acid and the separation purify reaction product. The process features the catalyst being H-type strong acid cationic exchange resin, which is the copolymer of sulfonated coal and sulfonated styrene or sulfonated phenolic resin; the benzene substitute being resorcin, catechol, o-methoxyphenol, m-methoxyphenol, veratrole, m-dimethoxyl benzene, o-ethoxyphenol, m-ethoxyphenol, o-diethoxyphenol or m-diethoxyphenol; and introduction of nitrogen during synthesis. The present invention has advantages of no corrosion of strong acid and the reuse of unreacted material after filtering.

Description

Technical field [0001] The present invention relates to an amide derivative, in particular to a method for synthesizing an amide derivative. technical background [0002] Amide derivatives have a wide range of applications, one of which is used in antifouling coatings. It usually uses a strong acid as a reaction catalyst to react N-hydroxymethyl fatty acid amide with the ortho or meta disubstituted benzene to form the corresponding amide derivatives. The British Patent No. 695529 reported that in the ethanol saturated solution of hydrogen chloride, the corresponding amide derivative was prepared by the reaction of o-methoxyphenol with N-hydroxymethyl saturated or unsaturated aliphatic amide containing 6 to 12 carbon atoms. ——N-(4-hydroxy-3-methoxybenzyl) fatty-based amide. U.S. Patent No. 1503631 reported the preparation of corresponding amide derivatives by reacting o-methoxyphenol with N-hydroxymethyl saturated or unsaturated fatty amides containing 6-12 carbon atoms in a conce...

Claims

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Application Information

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IPC IPC(8): C07C231/08C07C233/16C07C233/24
Inventor 于良民徐焕志
Owner OCEAN UNIV OF CHINA
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