34 results about "Cycloheptanone" patented technology

The invention relates to a 6,7-dihydro-5H-diphenyl[a,c]cyclohepta-5-ketone compound and a preparation method thereof. A formula of the compound is as shown in the specification. O-bromoaryl methanol, aryl ethanone, [Ir(cod)Cl]2, a palladium salt, a sliver salt, 1,1'-binaphthyl-2,2'-bisdiphenylphosphine and alkaline are taken and added into an organic solvent, heated and refluxed in the presence of an N2 gas, filtered, evaporated and re-crystallized after the reaction is ended to obtain the 6,7-dihydro-5H-diphenyl[a,c]cyclohepta-5-ketone compound. The 6,7-dihydro-5H-diphenyl[a,c]cyclohepta-5-ketone compound is synthesized by one step, wherein the reaction substrate scope is wide, the yield is high, the reaction is economical and efficient, and the application prospect is wide.

The invention discloses a camphor-based fluorescent probe for detecting hydrazine and a preparation method thereof. The camphor-based fluorescent probe is: 4-(4′-dimethylaminophenyl)-8,9,9-trimethyl-5,6,7,8-tetrahydro-5,8-endomethylene Quinazoline-2-amine. The present invention utilizes the natural renewable resource camphor as a raw material to condense with p-dimethylaminobenzaldehyde to generate 3-(4'-dimethylaminobenzylidene)-1,7,7-trimethylbicyclo[2.1.1 ]heptane-2-one; 3-(4′-dimethylaminobenzylidene)-1,7,7-trimethylbicyclo[2.1.1]heptane-2-one and then carry out condensation cyclization with guanidine hydrochloride , to obtain 4-(4'-dimethylaminophenyl)-8,9,9-trimethyl-5,6,7,8-tetrahydro-5,8-methanoquinazoline-2- amine. The compound can specifically react with hydrazine to emit significantly enhanced blue fluorescence, and can be used as a fluorescent probe for the detection of hydrazine, and has good practical value.

The invention discloses a method for detecting Fe 2+ The camphor-based enhanced fluorescent probe and its preparation method and application. The fluorescent probe is N,N-dimethyl-4-(3-(4,7,7-trimethyl-3-oxybicyclo[2.2.1]hept-2-enyl)prop-1-ene ‑1‑yl) aniline oxide. The present invention utilizes camphor as raw material, carries out condensation reaction with 4-dimethylaminocinnamaldehyde, obtains 3-(3-(4-(dimethylamino)phenyl) allylidene)-1,7,7-trimethyl 3-(3-(4-(dimethylamino)phenyl)allylidene)-1,7,7-trimethylbicyclo[2.1.1] Heptyl-2-one is oxidized with m-chloroperoxybenzoic acid to obtain N,N-dimethyl-4-(3-(4,7,7-trimethyl-3-oxybicyclo[2.2.1] Hep-2-enyl)prop-1-en-1-yl)aniline oxide. The compound can specifically recognize Fe 2+ , under 365nm ultraviolet light, the fluorescence of the solution changes from colorless to red, so it can be used to detect Fe 2+ The enhanced fluorescent probe has a detection limit of 8.3nM and a response time of 40s, which has a good application prospect.

The invention discloses a compound with azadibenzocycloheptanone as the core and its application in organic electroluminescent devices. This type of compound takes azadibenzocycloheptanone as the core, and the material is not easy to crystallize, and has the characteristics of good film formation and thermal stability; at the same time, it has a smaller triplet state than dibenzocycloheptanone. It is different from the singlet state energy, and can make full use of the triplet state energy. When the compound of the present invention is used as a light-emitting layer material of an OLED light-emitting device, the current efficiency, power efficiency and external quantum efficiency of the device are greatly improved; at the same time, the life of the device is significantly improved.

The invention relates to an artificial synthetic method of a harringtonine C-ring intermediate. According to the method, 3,4-methylenedioxyphenethylamine (compound I) as a raw material is subjected to acylation in alkaline conditions to obtain N-acylated-3,4-methylenedioxyphenethylamine (compound II), which is then reacts with halogenated acetic acid or halogenated acetic acid derivative to generate N-acylated-3,4-methylenedioxyphenethylamine acetic acid (compound III); and the compound (III) is catalyzed by Lewis acid to generate intramolecular Friedel-crafts acylation reaction to obtain N-acyl-3,4-metheneoxybenzo-3-N-cycloheptanone, namely C ring of harringtonine. In the preparation process, products of each step are purified by washing and recrystallization; and the method has simple operation, total yield of 87.4%, and good industrial prospect.

The compound “2-((4-nitrophenyl)amino)-6,7,8,9-tetrahydro-3H-cyclohepta[4,5]thieno-[2,3-d]pyrimidin-4(5H)-one” and method of synthesizing it, wherein the compound is effective to inhibit the growth and proliferation of human liver cancer cells HepG2. The compound has an inhibitory concentration value (IC50) of 0.7 μg, compared to reference medication Doxorubicin that has an (IC50) value of 1.2 μg. It further surpasses that reference medication Doxorubicin at all tested concentraions. The method includes the steps of: preparing a first compound of cycloheptanone, ethylcyanoacetate, sulfur, ethanol and diethyl amine; preparing a second compound by heating of the first compound with excess of hydrazine hydrate in absolute ethanol as solvent; and preparing the effective compound of the invention by reaction of the second chemical compound with 4-nitrophenylisothiocyanate in dry dimethylformamide as solvent.

The invention discloses a method for preparing hinokitiol. The method includes the steps of conducting an addition reaction on bromoform and an initial raw material compound, namely cyclohexene, to obtain a first compound, namely 7,7-dibromo bicyclo[4.1.0]heptane; the first compound is subjected to an oxidization reaction to obtain a second compound, namely 3,7,7-tribromo bicyclo[4.1.0]heptyl-2-ketone; the second compound is subjected to a substitution reaction to obtain a third compound, namely 7,7-dibromo-3-hydroxy bicyclo[4.1.0] heptyl-3-alkene-2-ketone; the third compound is subjected to aring enlargement reaction to obtain a fourth compound, namely 4-bromo-2-hydroxy cycloheptyl-2,4,6-triene-1-ketone; the fourth compound is subjected to an alkylation reaction to obtain hinokitiol.

The compound “2-((4-nitrophenyl)amino)-7,8,9,10-tetrahydro cyclohepta[4,5]thieno[2,3-d][1,3,4]thiadiazolo[3,2-a]pyrimidin-11(6H)-one” and method of synthesizing it, wherein the compound is effective to inhibit the growth and proliferation of human liver cancer cells HepG2. The compound has a higher efficiency to inhibit the growth and proliferation of these cells as it has an inhibitory concentration value (IC50) of 0.7 μg, compared to reference medication Doxorubicin that has an (IC50) value of 1.2 μg. It further surpasses that reference medication at all tested concentrations. The method includes the steps of: preparing a first compound of cycloheptanone, ethylcyanoacetate, sulfur, ethanol and diethylamine; preparing a second compound by heating of the first compound with excess of hydrazine hydrate in absolute ethanol as solvent; preparing a third compound by heating the second compound with carbon disulphide in dry pyridine; and preparing the compound of the invention by reacting the third compound with 4-nitrophenylisothiocyanate in dry N,N-methylformamide as solvent.

The invention relates to a method for preparing a class of ultraviolet absorber of alpha, alpha'-di(substituted benzilidene)ring ketone, in which various alpha, alpha'-di(substituted benzilidene)ring ketone compounds, alpha, alpha'-di(substituted benzilidene)cyclohexanones compounds and alpha, alpha'-di(substituted benzilidene)cycloheptanone compounds are generated through taking mixed solution of concentrated sulfuric acid with acetic as reaction solution and reacting under room temperature condition. The ultraviolet absorber of alpha, alpha'-di(substituted benzilidene)ring ketone compounds has stable chemical properties, can intensely absorb ultraviolet, in which its absorption range is 230-400n, and it can be used as wide spectrum ultraviolet absorbent.

A synthesis method of intermediate cycloheptanone of a guanethidine sulfate drug comprises the steps as follows: (i) 500-600 ml of water, 1.5 mol of metal powder and a phosphoric acid solution with the mass percentage being 40% -50% are added to a reaction vessel equipped with a stirrer, a thermometer and a dropping funnel, the temperature of the solution is controlled to be 60-70 DEG C, 1.2 mol of nitromethylcyclohexanol is added dropwise, the temperature of the solution is maintained to be 40-50 DEG C after addition, 30 mL of a sulfuric acid solution with the mass percentage being 40%-45% is added at an interval of 30 min and is added 3 times altogether, the pH of the solution is maintained to be 3-4 for 1 h, the filtrate is an aminomethyl cyclohexanol sulfate solution, and the filter cake is washed with a solvent and used for the next batch; (ii) pH of the solution is adjusted with sulfuric acid to be 2-3, the solution temperature is reduced to 2-5 DEG C, 1.5-2 mol of a sodium sulfite solution is added slowly and dissolved in 200 ml of water, the temperature is increased to 30-35 DEG C, distillation is performed through steam until no oily substances are distilled off, an oil layer is separated, a water layer is extracted with a solvent for 10-15 times, the oil layer and the solvent layer are combined, a solvent is distilled off under atmospheric pressure, distilling under reduced pressure is performed, a fraction at 65-70 DEG C is collected, and cycloheptanone is obtained.

The invention relates to a method for preparing a class of ultraviolet absorber of alpha, alpha'-di(substituted benzilidene)ring ketone, in which various alpha, alpha'-di(substituted benzilidene)ring ketone compounds, alpha, alpha'-di(substituted benzilidene)cyclohexanones compounds and alpha, alpha'-di(substituted benzilidene)cycloheptanone compounds are generated through taking mixed solution of concentrated sulfuric acid with acetic as reaction solution and reacting under room temperature condition. The ultraviolet absorber of alpha, alpha'-di(substituted benzilidene)ring ketone compounds has stable chemical properties, can intensely absorb ultraviolet, in which its absorption range is 230-400n, and it can be used as wide spectrum ultraviolet absorbent.

The invention belongs to the technical field of green pesticides, and discloses a new method for synthesizing flea aggregation pheromone. In the method, cycloheptanone (2) is used as the starting material, first bromination reaction with NBS occurs, and then elimination reaction occurs under the alkaline conditions of lithium bromide and lithium carbonate to obtain cycloheptenone 3, which is then catalyzed by copper. Asymmetric Michael addition reaction to obtain chiral methylcycloheptanone 4; then react with methyl iodide to obtain trimethylcycloheptanone 5. 5 undergoes an aldol condensation reaction with trimethylsilylbutenone under the catalysis of LDA , the diketone 6 was obtained, and finally the folic acid aggregation pheromone 1 was obtained by Robinson cyclization reaction. The invention utilizes the asymmetric Michael addition reaction for the first time to construct the chiral methyl group of the condensed pheromone, and has the advantages of simple synthesis route, easy operation and the like.

The present invention relates to a dibenzoxepanone compound derived from marine fungus WH4-2 and its preparation method and application. The marine fungus Tachybacterium stipe in the present invention has high-efficiency anti-Vibrio parahaemolyticus activity, and The yield of the active substance "dibenzoxepanone compounds containing isopentenyl group" is relatively large, and it is expected to be used in the development of new anti-Vibrio parahaemolyticus drugs. In further activity analysis, it was found that this type of compound also has anti- The activities of Bacillus subtilis, methicillin-resistant Staphylococcus aureus and Enterococcus faecium are expected to be developed into a class of broad-spectrum antibacterial drugs.

The present invention is starch / C4-C8 cyclic monomer grafted copolymer and its preparation process. Starch of corn, beans, potato and grains in grain size of 1-20 microns or modified starch in 1-60 portions and one or several C4-C8 cyclic monomer p-dioxy cyclohexanone, 1, 5-dioxy suberyl-2-one, gamma-butyrolactone, beta-butyrolactone, delta-valerolactone, epsilon-caprolactone, diglycolide and lactide in 40-99 portions react in a reaction bottle under the protection of inert gas and in the presence of catalyst in 0.01-5 portions at 60-150 deg.c for 10-48 hr to produce grafted copolymer. The unreacted monomer and homopolymer are extracted separately with solvent, the product is vacuum dried to constant weight, and the monomer converting rate, grafting rate and grafting efficiency are measured.

The compound “2-((4-nitrophenyl)amino)-7,8,9,10-tetrahydro cyclohepta[4,5]thieno[2,3-d][1,3,4]thiadiazolo[3,2-a]pyrimidin-11(6H)-one” and method of synthesizing it, wherein the compound is effective to inhibit the growth and proliferation of human liver cancer cells HepG2. The compound has a higher efficiency to inhibit the growth and proliferation of these cells as it has an inhibitory concentration value (IC50) of 0.7 μg, compared to reference medication Doxorubicin that has an (IC50) value of 1.2 μg. It further surpasses that reference medication at all tested concentrations. The method includes the steps of: preparing a first compound of cycloheptanone, ethylcyanoacetate, sulfur, ethanol and diethylamine; preparing a second compound by heating of the first compound with excess of hydrazine hydrate in absolute ethanol as solvent; preparing a third compound by heating the second compound with carbon disulphide in dry pyridine; and preparing the compound of the invention by reacting the third compound with 4-nitrophenylisothiocyanate in dry N,N-methylformamide as solvent.

The present invention relates to the new preparation process of 8-chloro-10, 11-dihydro-4-aza-5H-diphenyl[a, d]-5-cycloheptanone as the important intermediate of 2G non-calmative antihistamine loratadine. The preparation process includes successively the chemical reaction of the compound in expression (2) and phosphorus-containing reagent in solvent, the direct catalytic Friedel-Crafts reaction, and final hydrolysis to obtain target product in the same reactor. The synthesis process of the present invention has less reaction steps and simple operation, high product purity, and is suitable for industrial production.