504-02-9Relevant articles and documents
Method for preparing 1, 3-cyclohexanedione
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Paragraph 0026-0032, (2021/09/04)
The invention discloses a method for preparing 1, 3-cyclohexanedione. The method comprises the following steps: 1) dissolving acetylacetone and a catalyst in a solvent, adding acrylate into a constant-pressure dropping funnel, and dropwise adding acrylate into a reaction system, after drop-by-drop adding, heating to 60-80 DEG C, and continuously reacting for 0.5-1 hour; and 2) after the reaction is finished, cooling to 40 DEG C, adding a solid condensing agent, heating the reaction liquid to 40-50 DEG C, continuously reacting for 1-1.5 hours, concentrating under reduced pressure to remove the solvent and methyl acetate and other low-boiling-point byproducts generated by the reaction, then adding a small amount of water, adjusting the pH value to 1-2 by using hydrochloric acid (1.1-1.2 equivalent), cooling to separate out a product, centrifuging, leaching by using a small amount of ice water, carrying out pulping treatment by using ethyl acetate, filtering and drying to obtain the 1, 3-cyclohexanedione product.
Preparation method of 1,3-cyclohexanedione
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Paragraph 0013; 0026-0030; 0036-0045; 0061, (2020/06/09)
The invention relates to the technical field of chemical synthesis, in particular to a preparation method of 1,3-cyclohexanedione. The preparation method of the 1,3-cyclohexanedione comprises the following steps: with 1,3-acetonedicarboxylic ester and acrylate as raw materials, carrying out condensation and cyclization under the action of a base catalyst to prepare an intermediate; carrying out hydrolysis decarboxylation on the intermediate to obtain a crude product; and recrystallizing the crude product to obtain the 1,3-cyclohexanedione. The preparation method of the 1,3-cyclohexanedione hasthe advantages that process conditions are convenient to realize, post-treatment operation process is simple, yield is as high as 90.9%, reaction selectivity is high, production efficiency is high, operation safety is high, pollution is small, and the preparation method is suitable for industrial scale production.
Reversible chemoselective transetherification of vinylogous esters using Fe-catalyst under additive free conditions
Parvathalu, Nenavath,Agalave, Sandip G.,Mohanta, Nirmala,Gnanaprakasam, Boopathy
, p. 3258 - 3266 (2019/03/26)
An additive/Br?nsted acid/base free, highly efficient and chemoselective transetherification of electron deficient vinylogous esters and water mediated de-alkylation using an earth-abundant Fe-catalyst under very mild reaction conditions is described. This reaction is highly selective to primary alcohols over secondary alcohols, has good functional group tolerance, is scalable to gram scale and a purification free sequential transetherification in a continuous flow mode is demonstrated.