41 results about "Cyclononane" patented technology

The invention discloses a preparation method of heavy metal cadmium artificial antigen, which applies 2-S-(4- aminobenzene)-1, 4, 7, 10 tetraazacyclo cyclononane-1, 4, 7, 10-acetate tetrahydrate(p-NH2-Bn-DOTA, DOTA for short) as cheating agent, and couples cadmium ion chelating agent composite with carrier protein bovine serum albumin BSA or egg albumin OVA; thus the artificial antigen is prepared. The method adds the sodium borohydride processing step on the basis of traditional method, and improves the coupling efficiency and antiserum titre. The invention further discloses an application ofDOTA in preparation of the heavy metal cadmium artificial antigen.

The invention relates to an improved synthesis process of an antihypertensive drug irbesartan intermediate 2-butyl-1,3-diazaspiro[4.4]nonane-1-en-4-one. Cyclopentanone undergoes an addition reaction to obtain 1-aminocyclopentyl cyanide. The cyanide is first acylated, then hydrolyzed and cyclized under alkaline conditions to obtain the product. The positive effect of the present invention is that the first hydrolysis, then acylation and cyclization reported in the prior art is improved to first acylation, then hydrolysis and cyclization, each step does not go through the separation process, and the "one pot method" is realized Production. The operation process is simplified, the product yield is improved, the product quality is guaranteed, the production cost is reduced, and it is more conducive to large-scale industrial production.

The invention relates to a cycloalkane catalytic oxidation method promoted by iron porphyrin. O2 is taken as an oxidant, Co (II) porphyrin and Mn (II) porphyrin are taken as main catalysts, and Fe (II) porphyrin is taken as a cocatalyst to carry out reacting at a temperature of 100-160 DEG C and pressure of 0.8-2.0MPa under a solvent-free condition to realize catalytic oxidation of cycloalkanes. The cycloalkanes mainly comprise cyclopentane, cyclohexane, cycloheptane, cyclooctane and cyclononane, and the corresponding oxidation products mainly comprise cycloalkyl alcohols, cycloalkyl ketones and alkyl diacids. The cycloalkane catalytic oxidation method has the advantages of high selectivity of cyclopentanone, cyclohexanol, cycloheptanone and cyclooctanone, small catalyst consumption and simple operation, and environmental friendliness is achieved by taking clean O2 as the oxidant. The disclosesd cycloalkane catalytic oxidation method promoted by iron porphyrin is a cycloalkane catalytic oxidation method with high product selectivity, simple operation and environmental friendliness.

The invention provides a new synthesis method of 9-boron bicyclo (3,3,1)-nonane (9-BBN). 1,5-cyclooctadiene and borane are taken as raw materials, a reaction is carried out in a tetrahydrofuran solvent, and the 9-boron bicyclo (3,3,1)-nonane (9-BBN) is synthesized while yield is as high as 98%. The new synthesis method comprises the following steps of adding a smashed 4A molecular sieve, tetrahydrofuran, 1,5-cyclooctadiene and zirconium tetrachloride into a reaction flask, stirring for 1 hour, dropwise adding a dimethyl sulfide complex of borane at the temperature about 0 DEG C, carrying out a reflux reaction for 4 hours after dropwise addition is completed to obtain a product, cooling the obtained product to 0 DEG C and preserving heat for 3 hours, and filtering to obtain a 9-boron bicyclo (3,3,1)-nonane (9-BBN) solid product. The new synthesis method of the 9-boron bicyclo (3,3,1)-nonane (9-BBN) has the advantages of high yield, low cost, high product purity, easy operation, is beneficial to industrialization and has a good application prospect.

The invention discloses a degradable photoresist resin monomer synthesized from dimethyl bicyclo [3.3. 1] nonane diketone and a synthesis method of the resin monomer. The structural formula of the resin monomer is shown in the specification, wherein R1 is a saturated alkane or a cycloalkane, and R2 is hydrogen or methyl. The synthesis method comprises the following steps: reacting (1R, 4R, 5S, 6S)-4, 6-dimethyl bicyclo [3.3. 1] nonane-2, 8-dione (I) with an alkyl Grignard reagent or a cycloalkyl Grignard reagent under the protection of inert gas to obtain an intermediate (II); reacting the intermediate (II) with acryloyl chloride or methacryloyl chloride under an alkaline condition to obtain a resin monomer (III); polymer resin formed by polymerizing the resin monomer provided by the invention and other resin monomers has better etching resistance, is beneficial to improving the edge roughness of a developed pattern, and greatly improves the resolution of a photoetching pattern.

The invention discloses a photoresist resin monomer synthesized from 3-ethylbicyclo[3.3.1]nonane-2,4-dione, and a synthesis method thereof, and belongs to the technical fields of chemical synthesis and photoetching. The structural general formula of the photoresist resin monomer is represented by formula I shown in the description; and in the formula I, R1 is saturated alkane or cycloalkane, and R2 is hydrogen or a methyl group. The synthesis method comprises the following steps: carrying out a Grignard reaction on 3-ethylbicyclo[3.3.1] nonane-2,4-dione and an alkyl Grignard reagent or a cycloalkyl Grignard reagent under the protection of an inert gas, adding water for quenching after the Grignard reaction is finished, and carrying out post-treatment purification to obtain an intermediate;and carrying out an esterification reaction on the intermediate and acryloyl chloride or methacryloyl chloride, and carrying out post-treatment purification after the esterification reaction is finished in order to obtain the resin monomer. The resin monomer is a degradable resin monomer, and polymer resin containing the resin monomer has good etching resistance and can improve the resolution ofphotoresist photoetching patterns.

The invention discloses a preparation method of heavy metal zinc artificial antigen, which applies 2-S-(4- aminobenzene)-1, 4, 7, 10 tetraazacyclo cyclononane-1, 4, 7, 10-acetate tetrahydrate(p-NH2-Bn-NOTA, NOTA for short) as cheating agent, and couples mercury ion chelating agent composite with carrier protein bovine serum albumin BSA or egg albumin OVA; thus the artificial antigen is prepared. The method adds the sodium borohydride processing step on the basis of traditional method in the past, and improves the coupling efficiency and antiserum titre. The invention further discloses an application of NOTA in preparation of the heavy metal zinc artificial antigen.

The invention discloses a preparation method of heavy metal mercury artificial antigen, which applies 2-S-(4- aminobenzene)-1, 4, 7, 10 tetraazacyclo cyclononane-1, 4, 7, 10-acetate tetrahydrate(p-NH2-Bn-NOTA, NOTA for short) as cheating agent, and couples mercury ion chelating agent composite with carrier protein bovine serum albumin BSA or egg albumin OVA; thus the artificial antigen is prepared. The method adds the sodium borohydride processing step on the basis of traditional method in the past, and improves the coupling efficiency and antiserum titre. The invention further discloses an application of NOTA in preparation of the heavy metal mercury artificial antigen.

The invention discloses 2-nitro-2-aza adamantane-4, 6, 8-triol trinitrate and a preparation method of the 2-nitro-2-aza adamantane-4, 6, 8-triol trinitrate. According to the method, 9-hydroxyl bicyclo [3.3. 1] nonane-2, 6-diketone is used as a raw material, the 2-nitro-2-azaadamantane-4, 6, 8-triol trinitrate is finally synthesized through the steps of hydrazone formation, elimination, epoxidation, cyclization, acetylation, nitration and the like, the compound has higher density and energy, the synthesis method is simple, the yield is high, and the performance is stable.

The invention provides a method for preparing a moxifloxacin intermediate (S, S)-2, 8-diazabicyclo [4, 3, 0] nonane, and relates to the technical field of organic synthesis. According to the method, the azaphthalide is used as a raw material, and due to the ring structure of the azaphthalide, the other two non-corresponding chiral isomers which are not needed in chiral reduction are almost not generated; the chiral purity of the intermediate obtained through reduction is very high, resolution is not needed, and (S, S)-2, 8-diazabicyclo [4, 3, 0] nonane can be obtained directly through ammonolysis, reduction, chlorination and cyclization subsequently. According to the method provided by the invention, chiral resolution is not needed, the process is simple, the process steps are short, the cost is low, and the product is high in chiral purity and high in total yield. Furthermore, in the subsequent product salifying and refining step, carboxylic acid with a chiral structure does not need to be used for salifying, and common achiral carboxylic acid can be used for refining, so the product purity is further improved.

A substituted oxyheteroarylnonane-2-one compound used for preparing cell cycle depressant, cell wither inducer and antineoplastic medicine isprepared from streptomyces flavorectus.

The invention belongs to the technical field of optical fibers, and particularly relates to an h-GI-POF high-temperature optical fiber and a preparation method thereof. The h-GI-POF high-temperature light-guide fiber comprises an inner core layer and an outer skin layer, the inner core layer and the outer skin layer are arranged in a concentric structure, the inner core layer and the outer skin layer are composed of high polymers with different refractive indexes, the high polymers are formed by copolymerization of perfluorodioxolane and perfluoro dioxin bicyclononane, and the refractive indexof the inner core layer is larger than that of the outer skin layer. The inner core layer is integrally formed by five core layers of which the refractive indexes are gradually reduced from the coreto the outside, and the outer skin layer is formed by a single-layer skin layer, so that the transparency reaches 98% or above, the glass transition temperature Tg exceeds 150 DEG C, and the high-temperature optical fiber is suitable for ultra-high-speed communication. Compared with the SI-POF in the prior art, six layers of core materials are used, and each core layer has a gradual change refractive index, so that the incident light transmission delay is shorter than that of the common SI-POF, the signal transmission bandwidth is larger, and the transmission speed is higher.

The invention provides a synthesis method of 1, 4, 7-triazacyclononane. The preparation method comprises the step of: carrying out condensation ring-closure reaction on N, N'-bis (2-chloroethyl) ethylenediamine hydrochloride and ethylenediamine at low temperature to obtain 1, 4, 7-triazacyclononane. According to the method, the reaction temperature ranges from -50 DEG C to -30 DEG C, and the molar ratio of N, N'-bis (2-chloroethyl) ethylenediamine hydrochloride to ethylenediamine is 1: (0.95-1). 4-dimethylaminopyridine (DMAP) is adopted as an acid-binding agent, and the molar ratio of the DMAP to the N, N'-bis (2-chloroethyl) ethylenediamine hydrochloride is (3.9-4.1): 1. Carbon tetrachloride is selected as a reaction solvent, and the mass ratio of the carbon tetrachloride to the N, N'-bis (2-chloroethyl) ethylenediamine hydrochloride is 2: 1. According to the process, other side reactions can be effectively avoided, the highest reaction yield can reach 78% or above, and the product purity can reach 94% or above.

The invention discloses a reparation method of a 1,6-dioxaspiro [4, 4] nonane-3,8-diene derivative. The preparation method comprises the following steps: 1) adding isonitrile, acetylenic esters and carbon dioxide in a 25 ml round-bottom flask, and stirring vigorously under certain conditions; and 2) after the reaction, conducting reduced pressure distillation to remove the solvent and conducting column chromatography isolation by using petroleum ether-acetone as an eluent to obtain a product. The invention finds for the first time a multicomponent compound with two carbon oxygen double bonds of carbon dioxide participating at the same time; and the method has the advantages of simple reaction operations, convenient posttreatment, mild conditions and operation conditions of atmospheric pressure and no catalysis.

The invention relates to the technical field of organic chemical synthesis, and relates to a method for synthesizing 5-fluoro-1-azabicyclo[3, 2, 2]nonane and derivatives thereof. The preparation method comprises the following steps: reacting a 4-(hydroxymethyl)quinuclidine derivative with a fluorinating reagent at normal temperature, rearranging one six-membered ring of a quinine ring to obtain afluorine substituted product of a seven-membered ring, carrying out extraction, solvent removal and concentration on a reaction mixture, and carrying out column chromatography separation or sublimation to obtain pure 5-fluoro-1-azabicyclo[3, 2, 2]nonane and derivatives thereof. The 5-fluoro-1-azabicyclo[3, 2, 2]nonane and the derivative thereof are obtained through one-step synthesis by reacting the 4-(hydroxymethyl)quinuclidine derivative with the fluorinating reagent, and the method is discovered for the first time. The synthesis method is simple, has few synthesis steps, is easy to separate, and can realize large-scale synthesis of target products.

The invention discloses a synthesis method of 1,4-bis(p-toluenesulfonyl)trinitrocyclononane. The synthesis method comprises the following steps: with 1,4-bis(p-toluenesulfonyl)-7-benzoyltrinitrocyclononane as a substrate, removing a protecting group of a benzoyl group under an alkaline condition, and conducting a reaction under the condition that two p-toluenesulfonyl groups do not participate in the reaction so as to obtain the 1,4-bis(p-toluenesulfonyl)trinitrocyclononane. Reaction conditions are that a reflux reaction is adopted and reaction time is 10-36 hours. Compared with the prior art, the synthesis method of the invention has the following beneficial effects: the use of a large amount of inorganic acid and organic acid is avoided, and the problems of safety, environmental protection and the like are effectively guaranteed essentially; and reaction yield can be up to 90% or above.

The invention discloses a quinolone analogue and a preparation method and application thereof.The preparation method comprises the steps that S, S-2, 8-diazo-bicyclo [4.3. 0] nonane is dissolved in an organic solvent, and organic alkali is added; dissolving di-tert-butyl dicarbonate in an organic solvent, and dropwise adding into the reaction system to react to obtain a compound 1; dissolving the compound 1, slowly adding sodium hydride at 0-10 DEG C, and uniformly dispersing; the preparation method comprises the following steps: adding a compound 1 into a reaction system, dropwise adding a 1-cyclopropyl-6, 7-difluoro-8-methoxy-1, 4-dihydro-4-oxo-3-quinoline carboxylic acid solution into the reaction system, and reacting to obtain a compound 2; and dissolving the compound 2, and adding acid for reaction to obtain a compound 3, namely the target quinolone analogue. The preparation method of the quinolone analogue is simple and easy to implement, and the quinolone analogue can be prepared on a large scale. When the quinolone analogue is used for detecting related substances of moxifloxacin hydrochloride and preparations thereof, the quality of moxifloxacin hydrochloride can be further improved, the safety is improved, and the risk of medication is reduced.