- Method of using solid acid catalyst to synthesize amide-type cooling agent
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The invention belongs to the technical field of compound preparation, and discloses a method of using a solid acid catalyst to synthesize an amide-type cooling agent. According to the method, 2,2-diisopropyl propane nitrile, C1-C6 lower aliphatic alcohols, and water are taken as the raw materials; and under the action of a solid acid catalyst, thermostatic alcoholysis circular reactions are carried out in a fixed bed reactor. Solid acids are used to replace liquid acids, the problem that a large amount of low concentration acidic wastewater is generated in conventional cooling agent production is solved, the discharge of waste solid, waste gas, and wastewater is reduced, at the same time, the corrosion on production equipment is largely reduced; the method is green and environmentally friendly; a fixed bed reactor is adopted, an outer circulation type reaction technology is used, the alcoholysis process of converting cyano groups into N-alkyl amide is smoothly carried out, the lower aliphatic alcohols can be circularly used after being separated by a gas-liquid separator; the raw material waste is reduced, and continuous production is realized.
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Paragraph 0029-0032; 0037-0044; 0049-0060
(2019/10/04)
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- Synthetic method of cooling agent N,2,3-trimethyl-2-isopropyl butylamide
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The invention discloses a synthetic method of cooling agent N,2,3-trimethyl-2-isopropyl butylamide. The synthetic method comprises the following steps: (1) enabling methyl acetoacetate to react with 2-bromopropane under the condition of strong alkali to obtain 3,3-diisopropyl acetoacetate methyl ester; (2) enabling the obtained 3,3-diisopropyl acetoacetate methyl ester to react with ethylene glycol, so that keto-carbonyl groups are protected, hydrolyzing ester into hydroxyl in the presence of a reducing agent, then enabling the hydroxyl to react with p-methyl benzene sulfonic chloride, then removing parabensulphonate, and obtaining 3-isopropyl-4-methyl-2-pentanone; and (3) enabling the 3-isopropyl-4-methyl-2-pentanone to react with hydroxylamine hydrochloride, and then performing the beckmann rearrangement under an acid condition to obtain N,2,3-trimethyl-2-isopropyl butylamide. According to the method, the N,2,3-trimethyl-2-isopropyl butylamide is successfully obtained by virtue of methylation of ester groups and the Beckmann rearrangement, and a novel synthetic method is provided for synthesizing WS-3; and moreover, the method is high in yield and suitable for mass production.
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Paragraph 0020; 0021; 0024
(2018/05/16)
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- Lower primary alkanols and their esters in a Ritter-type reaction with nitriles. An efficient method for obtaining N-primary-alkyl amides
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N-Primary-alkyl amides RCONHR1 were obtained by a Ritter-type reaction of nitriles RCN with lower primary alkanols R1OH or their esters in the presence of acids.
- Lebedev, Mikhail Y.,Erman, Mark B.
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p. 1397 - 1399
(2007/10/03)
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- Method for making amides
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The invention relates to the manufacture of amide compounds provided through the reaction of nitrile compounds and a sulfate compound to form the related amide compound. In a preferred embodiment a diol or a triol is employed as a solvent, thereby increasing the yield of the product.
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- Method for making amides
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The invention relates to the manufacture of amide compounds provided through the reaction of nitrile compounds and a sulfate compound to form the related amide compound. In a preferred embodiment a diol or a triol is employed as a solvent, thereby increasing the yield of the product.
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- Acyclic carboxamides having a physiological cooling effect
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Compositions are disclosed having a physiological cooling action on the skin. The compositions contain, as the active ingredient, certain acyclic tertiary and secondary carboxamides.
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