46 results about "Adamantanecarboxylic acid" patented technology

The invention discloses a molybdenum-containing polyoxometalate and adamantane hybrid compound, which is prepared by connecting molybdenum-containing polyoxometalate and adamantane through a covalent bond. The preparation method comprises the following synthesis steps of: 1) performing amidation reaction on adamantane carboxylic acid serving as an initial raw material and trishydroxymethyl aminomethane to obtain N-trishydroxymethyl-adamantane carboxamide; and 2) reacting with the molybdenum-containing polyoxometalate to obtain the hybrid compound. By the invention, the molybdenum-containing polyoxometalate and the adamantine are connected through the covalent bond for the first time; and the synthesis method is simple and feasible, reaction conditions are easy to realize, purification is simple, and the yield is high. The hybrid molecule has potential application value in the aspects of medicines, lubricants, surfactants, catalysts and the like.

A method for preparing a magnesium adamantane carboxylate salt is provided. The method includes mixing a magnesium salt and a diamondoid compound having at least one carboxylic acid moiety to form a reactant mixture and hydrothermally treating the reactant mixture at a reaction temperature for a reaction time to form the magnesium adamantane carboxylate salt.

Embodiments of the present disclosure are directed towards methods for preparing mixed-metal oxide particles by heating adamantane-intercalated layered double-hydroxide (LDH) particles at a reaction temperature of from 400° C. to 800° C. to form mixed-metal oxide particles. The adamantane-intercalated LDH particles have a general formula [M_1-xAl_x(OH)₂](A)_x.mH₂O, where x is from 0.14 to 0.33, m is from 0.33 to 0.50, M is chosen from Mg, Ca, Co, Ni, Cu, or Zn, and A is adamantane carboxylate, and an aspect ratio greater than 100. The aspect ratio is defined by the width of an adamantane-intercalated LDH particle divided by the thickness of the adamantane-intercalated LDH particle. The mixed-metal oxide particles comprise a mixed-metal oxide phase containing M, Al or Fe, and carbon.

The invention relates to a method for separation and purification of an adamantanecarboxylic acid mixture, especially a method for separation and purification of 2-adamantanecarboxylic acid and 1-adamantanecarboxylic acid. Comprising the steps of esterification and separation, the method is characterized in that: in the esterification reaction, 98% sulfuric acid is employed as a catalyst, with the ratio of the catalyst to raw materials in a range of from 0.5-3:10, the reaction time is 15-140min, and the reaction temperature ranges from 55-70DEG C; then water and NaOH are added to make the pH value of the solution above 10, so that a water and an ester layer is separated. In the invention, the separation of 1-adamantanecarboxylic acid and 2-adamantanecarboxylic acid is realized through an esterification reaction, i.e. through the esterification differences between 2-adamantanecarboxylic acid and 1-adamantanecarboxylic acid. Therefore, not only is the method of the invention simple and practicable, but also the product generated after separation and purification has satisfying purity. Especially, residues from adamantanecarboxylic acid production can be fully utilized, so that the discharge of "three wastes" can be reduced and environmental pollution is prevented. With remarkable economic benefit and social benefit, the method of the invention is economical and environmental friendly.

A preparation method of a 2-(2-alkylphenoxy)pyridine derivative adopts a reaction of a 2-phenoxypyridine derivative and a primary bromoalkane compound. The method concretely comprises the following steps: directly adding the 2-phenoxypyridine derivative, the primary bromoalkane compound, a catalyst, an additive, an alkali and a solvent into a reaction device, stirring and heating the above added substances until the temperature is 90-130 DEG C, carrying out a reaction for 18-36 h, and separating the obtained product to obtain the 2-(2-alkylphenoxy)pyridine derivative, wherein the catalyst is dichloro(p-cymene)ruthenium dimer; the alkali is potassium carbonate or lithium carbonate; the additive is 1-adamantanecarboxylic acid or naphthenic acid; and the solvent is benzene or DMF or ethylene glycol dimethyl ether. The method has the advantages of easiness in obtaining of synthesis raw materials, simple process, and very good specificity of the reaction.

The invention discloses a method for synthesizing 3-amino-1-adamantanol. The structural formula of the 3-amino-1-adamantanol is as follows. Using adamantanecarboxylic acid as starting material, the method synthesizes the 3-amino-1-adamantanol according to the following reaction steps: bromate 3-amino-1-adamantanol is synthesized by way of bromination, modified curtius rearrangement and hydrolyzation, and finally, bromate is removed by a alkaline liquor treatment method, so that the 3-amino-1-adamantanol is obtained. The invention has the advantages of simple and easy operation, available materials, less reaction steps and high product yield.

The invention discloses a 7-alkyl-N-pyrimidylindoline compound and a synthesis method thereof. The 7-alkyl-N-pyrimidylindoline compound has a general structural formula shown in the description. The synthesis method comprises: adding an N-pyrimidylindoline compound and a vinyl cyclopropane compound into a reaction tube in an argon environment, adding 1-adamantanecarboxylic acid, [Cp*Rh(CH3CN)3](SbF6)2 and silver hexafluoroantimonate into the reaction tube, then adding methanol into the reaction tube, carrying out a reaction process at 80-120 DEG C for 12h, and then carrying out leaching, thinlayer chromatographic separation and drying to obtain a desired product. The metal ruthenium (III) is used as a catalyst and methanol is used as a reaction solvent so that the carbon-carbon bond cleavage of vinylcyclopropane and activation of a 7-site carbon-hydrogen bond of an indoline compound are realized. The long alkyl chain with double bonds realizes a further functionalization reaction. Thesynthesis method is simple and efficient and has good selectivity. The 7-alkyl-N-pyrimidylindoline compound is easy to purify.

The invention relates to a method for preparing adamantyl-containing unsaturated ester. The method for preparing the monomer comprises the following steps of: simultaneously adding hydroxyl acrylate and tertiary amine into organic solvent for stirring; dissolving adamantanecarboxylic acid chloride in the organic solvent, and slowly dripping the solvent in mixed solution to react at the temperature of between 0 and 5 DEG C; continuously stirring the solution for 5 hours after 3-hour dripping is completed; standing the mixture over-night; filtering the solution; and washing and drying the solution and performing rotary evaporation to obtain the adamantyl unsaturated ester. The preparation method has the advantages of simple and convenient experiment steps, easily controlled reaction process and reduction of possibility of generating side products, and easy realization of industrialization.

The invention discloses insecticidal and antiviral foliar fertilizer and a preparation method thereof. The preparation method comprises preparation of rimantadine hydrochloride, preparation of a saponin extract and preparation of foliar fertilizer, wherein the rimantadine hydrochloride is prepared by the following steps: carrying out heating reflux reaction on adamantanecarboxylic acid and thionylchloride, extracting benzene, slowly adding a benzene extract liquor into a three necked bottle containing trimethylaluminum and cerium formate for reaction, and then treating with ice water to obtain adamantane methyl ketone; adding hydroxylamine hydrochloride, alkali and alcohol for oximation into ketoxime, catalyzing by platinum-carbon for hydrogenation reduction, and then acidizing to form salt by hydrogen chloride gas, so as to obtain rimantadine hydrochloride. The preparation method has the beneficial effects that by preparing rimantadine hydrochloride with trimethylaluminum and ceriumformate, a previous route for synthesizing adamantane methyl ketone is changed, and mild reaction conditions, fewer by-products and high product yield are achieved; the foliar fertilizer prepared withrimantadine hydrochloride not only has insecticidal, antibacterial and antiviral effects, but also is capable of quickly supplementing foliar nutrition.

The invention belongs to the technical field of organic chemical industry surface activity, and particularly relates to synthesis of an adamantane-containing Gemini surfactant, wherein the adamantane-containing Gemini surfactant has a structural formula defined in the specification, R represents CnH2n+1, and n is 12,16 or 18. According to the present invention, the Gemini surfactant is obtained byusing 1-adamantanecarboxylic acid as a raw material through a three-step reaction, wherein the three-step reaction comprises that 1-adamantanecarboxylic acid and thionyl chloride are subjected to anacyl chlorination reaction to synthesize 1-adamantanecarbonyl chloride, the 1-adamantanecarbonyl chloride and 3,3'-iminobis(N,N-dimethylpropylamine) are subjected to an amidation reaction to prepare akey intermediate bis(N,N-dimethylpropylamine)adamantane-1-formamide, and finally the intermediate and a long chain brominated alkane are subjected to quaternization to form the adamantane-containingGemini surfactant. According to the present invention, the obtained adamantane-containing Gemini surfactant has characteristics of mild reaction condition, easily available raw materials and simple and easy-performing operation, and has potential application prospects in the fields of supramolecular chemistry, nanometer materials, special washing and the like.

Methyl 2,4,9-trithiaadamantane-7-carboxylate and a method for its manufacture is disclosed. The method reacts oxidized methyl triallyl acetate with a Lewis acid and a sulphuring agent.

The invention belongs to the field of organic synthesis and particularly relates to a synthesis method of 3-hydroxy-1-adamantanecarboxylic acid. In the method, with 1-adamantanecarboxylic acid being araw material and triethyl benzyl ammonium chloride (TEBAC) being a phase transfer catalyst, the 3-hydroxy-1-adamantanecarboxylic acid is prepared under alkaline conditions through hydroxylation withKMnO4. The new preparation method not only is reduced in cost and protects environment, but also is simple in operation and convenient in post-treatment. The method is high in yield, is simple in synthesis and is suitable for industrial production.

The invention provides a method for preparing 4-amino-adamantanecarboxylic acid. 4-carbonyl-adamantanecarboxylic acid, five to ten N of NH<3>/MeOH solutions and sodium borohydride are firstly weighed, the 4-carbonyl-adamantanecarboxylic acid and the NH<3>/MeOH solutions are added into a reaction vessel and stirred at room temperature, reaction liquid is cooled to -5 DEG C to 2 DEG C, the sodium borohydride is added, stirring is carried out for two to six hours, the reaction liquid is spin-dried, water is added for dissolution, stirring is carried out, PH is adjusted to five to six through hydrochloric acid, stirring continues, the reaction liquid is extracted two to five times through first organic solvents, and the first organic solvents are combined. After spin-drying, second organic solvents and water are added into solids for dissolution, stirring is carried out for four to ten hours at room temperature, suction filtration is carried out, and the 4-amino-adamantanecarboxylic acid is obtained after solid products are dried. No high-pressure vessel is adopted, reactions are carried out in a common vessel, no noble metal catalyst is adopted, cost is lowered, no hydrogen gas reduction is adopted, high operability is achieved, and the industrial application prospect is achieved.