Synthetic method for amide derivatives

A technology of amide derivatives and synthesis methods, which is applied in the field of amide derivatives, can solve the problems of strong acid corrosiveness of catalysts, difficulty in separating and reusing unreacted raw materials, etc., and achieve the effect of easy operation and corrosion avoidance

Inactive Publication Date: 2004-10-20
OCEAN UNIV OF CHINA
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  • Abstract
  • Description
  • Claims
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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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  • Synthetic method for amide derivatives
  • Synthetic method for amide derivatives

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Embodiment 1

[0009] The synthesis of embodiment 1.N-(4-hydroxyl-3-methoxy-phenylmethyl) acrylamide

[0010] Experimental procedure: (1) in 1000ml there-necked flask, add the guaiacol (o-methoxyphenol) of 50.8 grams (0.41mol), the N-methylol acrylamide of 40.4 grams (0.4mol), 200 grams of acid Treated 732-type cation exchange resin, then slowly add 400ml of absolute ethanol under stirring, and pass through N 2 (to prevent the hydroxyl group from being oxidized), the reaction was stirred at room temperature (about 30° C.) for 7-8 days.

[0011] (II) Filter the reaction mixture, wash the H-type cation exchange resin several times with absolute ethanol, and combine the washing solution and the mother liquor.

[0012] (III) The obtained liquid was evaporated to dryness under reduced pressure at 50°C, the residue was washed with ether, dried and then washed with water to obtain a crude product.

[0013] (IV) After dissolving the crude product with dilute lye, remove the insoluble matter by fil...

Embodiment 2

[0014] The synthesis of embodiment 2.N-(3,4-dihydroxy-benzyl) acrylamide

[0015] Experimental procedure: (1) in 1000ml there-necked flask, add the catechol of 44.0 grams (0.41mol), the N-methylolacrylamide of 40.4 grams (0.4mol), the 732 type cation after the acid treatment of 200 grams Exchange resin, then slowly add 400ml acetic acid under stirring, and pass into N 2 , the reaction was stirred at room temperature (about 30° C.) for 7-8 days.

[0016] (II) Filter the reaction mixture, wash the H-type cation exchange resin several times with acetic acid, and combine the washing solution and the mother liquor.

[0017] (III) The obtained liquid was evaporated to dryness under reduced pressure at 50°C, the residue was washed with ether, dried and then washed with water to obtain a crude product.

[0018] (IV) After dissolving the crude product with dilute lye, remove the insoluble matter by filtration, and slowly add dilute acid to adjust the pH to 2-3 to obtain a khaki-yello...

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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 invention relates to an amide derivative, in particular to a synthesis method of the amide derivative. technical background [0002] Amide derivatives have a wide range of applications, and antifouling coatings are one of them. It usually uses a strong acid as a reaction catalyst to react N-methylol aliphatic amides with benzene ortho- or meta-disubstituted products to generate corresponding amide derivatives. British Patent No. 695529 reported that in a saturated ethanol solution of hydrogen chloride, the corresponding amide derivatives were prepared by reacting o-methoxyphenol with N-methylol containing 6-12 carbon atoms of saturated or unsaturated aliphatic amides - N-(4-hydroxy-3-methoxybenzyl) fatty acid amides. U.S. Patent No. 1503631 reported that in the ethanol solution of concentrated sulfuric acid, the corresponding amide derivatives were prepared by reacting o-methoxyphenol with N-methylol containing 6-12 carbon atoms of saturated or u...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/08C07C233/16C07C233/24
Inventor 于良民徐焕志
Owner OCEAN UNIV OF CHINA
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