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Acidamide derivative preparation method

A technology of amide derivatives and catalysts, applied in the field of amide derivatives, can solve the problems of easy generation of waste acid or waste alkali, strong corrosion of catalyst strong acid or strong alkali, difficulty in separation and reuse, etc., to avoid corrosion and facilitate operation Effect

Inactive Publication Date: 2004-11-10
OCEAN UNIV OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The common disadvantage of these preparation methods is that the strong acid or strong base of the catalyst is extremely corrosive, and it is easy to produce waste acid or waste alkali, and it is difficult to separate and reuse unreacted raw materials.

Method used

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  • Acidamide derivative preparation method

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Effect test

Embodiment 1

[0006] The preparation of embodiment 1.N-(1-hydroxyl-2,2,2-trichloroethyl)acrylamide

[0007] Experimental procedure: (1) in 1000ml there-necked flask, add the acrylamide of 71.1 grams (1mol), 0.5 gram stopper phenothiazine, 15g Amberlyst35 (the strong acid cation of the H type that Shanghai Rohm and Haas Chemical Co., Ltd. produces Exchange resin) and 150 milliliters of methanol, nitrogen, after a few minutes, put the reaction bottle into 80-90 ℃ oil bath, then slowly drop into 100 milliliters of methanol solution of 181.5 grams of chloral hydrate under stirring, about 2 to 3 After the addition was completed within 1 hour, the reaction was continued with heating and stirring for 1 to 2 hours under the protection of nitrogen.

[0008] (II) Filter the reaction mixture, wash the H-type cation exchange resin several times with methanol, and combine the washing solution and the mother liquor.

[0009] (III) The obtained liquid was evaporated to dryness under reduced pressure at 5...

Embodiment 2

[0011] The preparation of embodiment 2.N-(1-hydroxyl-2,2,2-trichloroethyl)methacrylamide

[0012] Experimental procedure: (1) In a 1000ml three-necked flask, add 85.1 grams (1mol) of methacrylamide, 0.5 grams of phenothiazine, 15g of Amberlyst and 150 milliliters of methanol, and place the reaction bottle at 80-90°C after purging nitrogen for several minutes In an oil bath, slowly add 181.5 g of chloral hydrate in 100 ml of methanol solution dropwise under stirring, and the addition is completed in about 2 to 3 hours, and the reaction is continued with heating and stirring for 1 to 2 hours under the protection of nitrogen.

[0013] (II) Filter the reaction mixture, wash the H-type cation exchange resin several times with methanol, and combine the washing solution and the mother liquor.

[0014] (III) The obtained liquid was evaporated to dryness under reduced pressure at 50° C., and the crude product was obtained after drying.

[0015] (IV) Recrystallize the crude product fro...

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Abstract

A process for preparing amide derivant, comprises reacting fatty group amide with aldehydes in methyl alcohol or carbon tetrachloride or benzene or methylbenzene or dioxane or acetonitrile with the presence of catalyst, and separating the reaction product, characterized in that the catalyst is type H strong acidic positive ion exchange resin, the aldehyde is selected from the groups of paraformaldehyde, acetaldehyde, propionaldehyde, chloral, bromal, glyoxylic acid, 4-bromobenzaldehyde, 3-bromobenzaldehyde, hydrosulfide acetaldehyde, p-nitrobenzaldehyde, and 4-hydroxybenzaldehyde. The formula of the fatty group amide is described in the specification, wherein R 2 is saturated or unsaturated fatty group having 2-12 carbon atoms, the type H strong acidic positive ion exchange resin is sulphonated coal, sulfonated phenylethene copolymer or sulfonated phenol formaldehyde resin.

Description

technical field [0001] The invention relates to an amide derivative, in particular to a preparation method of the amide derivative. Background technique [0002] Chlorine-containing N-hydroxyalkylamide derivatives have a wide range of applications, such as rubber vulcanization accelerators, and their polymers are often used in fire retardants and marine antifouling coatings, etc., and are usually reacted with strong acids or strong bases during preparation Catalysts to react amides and aldehydes to generate corresponding N-hydroxyalkylamide derivatives. The British No. 835579 patent has reported that in benzene solvent, using a strong base such as trimethylamine as a catalyst, the unsaturated amide reacts with chloral to prepare the corresponding amide derivative——N-(1-hydroxyl-2,2,2 -trichloroethyl) unsaturated fatty amides. In a paper (Farafontova V.I., Podgornova, etc. reported in Zh.Prikl.Khim (Leningrad), 1975, 48 (1) 240-3 (RUSS)): under the catalysis of sodium methy...

Claims

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Application Information

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IPC IPC(8): C07C231/12
Inventor 徐焕志于良民张志明
Owner OCEAN UNIV OF CHINA
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