22945-27-3Relevant articles and documents
Synthesis process of gliclazide intermediate 2-formamide cyclohexanone
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Paragraph 0018-0042, (2021/04/17)
The invention provides a synthesis process of a gliclazide intermediate 2-formamide cyclohexanone, and relates to the technical field of synthesis of gliclazide intermediates. According to the synthesis process disclosed by the invention, after the reaction kettle is cooled in advance, the solvent xylene and the raw material urea are added and the catalyst tetrabutyl titanate is added, the spiro intermediate can be generated through high-selectivity catalysis along with the addition of cyclohexanone, and the reaction condition of high-temperature azeotropy is not needed; ketone can be hydrolyzed and removed only at a low temperature after heating, water adding and stirring are carried out; after xylene and residual cyclohexanone are removed from the filtrate through vacuum concentration, ethanol is used for dispersing the crude product of the 2formamide cyclohexanone, and sodium bicarbonate is used for neutralizing generated hydrogen ions, so that the neutral environment of the system is maintained, and a pure product of the 2-formamide cyclohexanone with high yield and purity is obtained after subsequent filtration and crystallization.
Synthesis method of cyclopentane-1,2-dicarboximide
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Paragraph 0030-0039, (2018/10/19)
The invention discloses a synthesis method of cyclopentane-1,2-dicarboximide. The synthesis method comprises the following steps: performing dehydration on cyclohexanone and urea as raw materials under the actions of a polymerization inhibitor and a water-carrying agent, heating, dropwise adding an acid liquor for hydrolyzing, adding an alcoholic solvent in the hydrolyzed solution, crystallizing,centrifuging, and drying to obtain cyclohexane-2-carboxamide, dissolving cyclohexane-2-carboxamide in halogenated hydrocarbon, performing halogenation under a halogenation reagent, performing cooling,crystallizing, hydrolyzing, centrifuging and drying to obtain a halide, dispersing the halide in an ammoniating solution for Favorskii rearrangement, sequentially performing cooling, crystallizing, centrifuging, washing and drying to obtain a rearrangement object, namely cyclopentane-1,2-carboxamide, finally adding a proper amount of catalysts, and after high temperature cyclization, performing reduced pressure distillation, performing refined crystallization, centrifuging, and drying, thereby obtaining cyclopentane-1,2-dicarboximide. The synthesis method has the advantages that the reactionstep is shortened, the environmental protection is benefited, the production cost is reduced, and the synthesis method is suitable for large-scale mass production.
Synthesizing process for improving yield of gliclazide intermediate 2-formamide cyclohexanone
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Paragraph 0020-0021, (2017/01/09)
The invention provides a synthesizing process for improving the yield of a gliclazide intermediate 2-formamide cyclohexanone. According to the invention, on the basis of an original process, a novel catalyst titanium(IV) isopropoxide is added into a reaction system, such that a synthesis yield is improved from 82% to 90% while product quality is improved. The process has significant economic benefits.
5',6',7',8'-Tetrahydro-1'H,3'H-spiro[cyclohexane-1,2'-quinazolin]-4'-one in Mannich reaction
Markov,Farat
, p. 925 - 930 (2013/01/15)
The Mannich aminomethylation of 5',6',7,'8'-tetrahydro-1'H,3'H- spiro[cyclohexane-1,2'-quinazolin]-4'-one leads to formation of a heterocyclic system containing an annelated azabicyclic fragment. Hydrolysis of the indicated spirans gives 3-azabicyclo[3.3.1]nonanes.
Process for the preparation of cyclohexanone-2-carboxamide
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, (2008/06/13)
This invention relates to an improved process for preparation of cyclohexanone 2-carboxamide which is in turn useful for preparing herbicides by condensation of one equivalent of urea with more than two equivalents of cyclohexanone, under controlled conditions of pH.